Document JJQ5ZbEv7q0MpvRzyBNzgB7KO

Study Title TENNESSEE RIVER VALLEY SAMPLES Author Mark E. Ellefson Revised Report September 12, 2003 Performing Laboratory 3M EnvironmentalLaboratory Building2-3E-09 935 BushAvenue SL Paul,MN 55106 Project Identification 3M Environmental Laboratory Study# E02-0443 Total Number of Pages 276 Report E02-0443 Tenn. RiverValley Samples TABLE OF CONTENTS List of Tables .....................................................................................................................................3. Study Information .............................................................................................................................4.. Summary ......................................................................................"......................................................5 Purpose ............................................................................................................................................6.. Test and Analytical Reference Substances.......................................................................................6. Test Systems....................................................................................................................................7.. Method Summaries ..........................................................................................................................8.. Preparatory Methods ........................................................................................................................8.. Sample Analysis ...............................................................................................................................1.. 1 Analytical Method .............................................................................................................................1..2 Analytical Results .............................................................................................................................1..3 Data Summary .................................................................................................................................2..0 Statistical Methods ...........................................................................................................................2..5 Statement of Conclusion ..................................................................................................................2.. 6 References .......................................................................................................................................2..6 List of Attachments...........................................................................................................................2..6 Signature Page.................................................................................................................................2..7 Attachment A: Analytical Method and SOP Deviations .....................................................................2. 8 Attachment B: Data Summary Tables..............................................................................................4.. 0 Attachment C: Sample Chromatograms ...........................................................................................6. 7 Attachment D: Sample Prep Sheets, Test Substance, and Test System Information.......................2 30 Attachment E: Notes to File................................................................................................................2 70 3M EnvironmentaLl aboratory Page 2 of 276 ReportE02-0443 i Tenn.RiverValleySamples LIST OF TABLES Table 1. Sample Location, Sample Type, and Analytical Data Summary. .................................... 5 Table 2: Characterization of the Test and Analytical Reference Substances ............................. .6 Table 3a. Description cf Fish Tissue Analyzed in this Study. ...................................................... .7 Table 3b. Description of River Water Analyzed in this Study .......... ............................................... .7 Table 3c. Description of River Sediments Analyzed in this Study .................................................... 7 Table 4a. Fish Tissue Sample Preparation Method .................................................................. .8 Table 4b. Preparation of Extracted Calibration Curves for the Fish Tissue. .................................. 9 Table 4c. Fish Tissue Analytical Data Quality Objectives ....................................................... .9 Table 4d. River Water Sample Preparation Method .................................................................. .9 Table 4e. River Water Sample Data Quality Objectives ............................................................. 10 Table 4f. River Sediment Sample Preparation Method .............................................................. 10 Table 4g. River Sediment Sample Data Quality Objectives ................................. 11 Table 5. Sample Analysis Information. .................................................................................. 11 Table 6a. PFOS Calibration Standard Reprocessing Summary ............................................... 14 Table 6b. FOSA Calibration Standard Reprocessing Summary .................................................. 15 Table 6c. PFOA Calibration Standard Reprocessing Summary .................................................. 16 Table 6d. PFHS Calibration Standard Reprocessing Summary ...................................................... 1 7 Table 6e. PFBS Calibration Standard Reprocessing Summary. .................................................. 18 Table 7a. Catfish Analytical Data ......................................................................................... 21 Table 7b. Large mouth and Small mouth Bass Analytical Data .............................................. .22 Table 7c. River Water Analytical Data .................................................................................. .2 3 Table 7d. River Sediment Analytical Data. ......................................................................... 24 Table 8. Sample Location, ,Sample Type, and Analytical Data Summary ..................................... 2 5 3M EnvironmentLaal boratory Page3 of 276 Report E02-0443 Tenn. River Valley Samples STUDY INFORMATION Requestor Dale L. Bacon 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 651-778-4736 Study Director Mark E. Ellefson 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 651-778-5405 Study Location Testing Facility 3M EnvironmentaLl aboratory Bldg.2-3E-09 935 BushAvenue St. Paul, MN 55106 WilliamK. Reagen, Laboratory Manager Mark L. Anderson,Analytical Chemist CindyM. Carlson,Analytical Chemist OgnjenkaKrupljaninA, nalytical Chemist ExperimentalDates SampleAnalysisInitiation2: 6 June2002 SampleAnalysisCompletion:12 November2002 Locationof Archives All originalraw data and the reporthave beenarchivedat the3M EnvironmentaLl aboratory accordingto 3M StandardOperatingProcedures.Remainingspecimenspertainingto the analyticalphase ofthis studywillbe archivedat the3M EnvironmentaLl aboratoryforas longas the qualityof the preparationaffordsevaluation. 3M EnvironmentaLl aboratory Page 4 of 276 ReportE02-0443 Tenn. River Valley Samples SUMMARY Fish, riverwater, and river sediment sampleswere collectedfrom three locations in the Tennessee River nearthe 3M Decatur, Alabamafacility. The samples were analyzed for perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), perfluorooctanoate (PFOA),-perfluorooctanesulfonylamide (FOSA), and perfluorooctanesulfonate (PFOS). The analyses were accomplishedby extracting the samples using Solid Phase Extraction (SPE) and then analyzingthem using HPLC-Electrospray/MassSpectrometry (HPLC/ES/MS). Sampling Location 1 (SL-1) was located downstreamof the 3M facility near Fox Creek at river mile 296. Sampling Location 2 (SL-2) was across the river from the 3M facility at river mile 301. Sampling location 3 (SL-3) was upstream from the 3M facility at river mile 307.5. Analyticalresults are presented in Table 1: Table1. Sample Location,SampleType,andAnalyticalDataSummary. Sampling Location& SpeciesSampled <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ1 <LLOQ <LLOQ <LLOQ 60.9 (6/6)z <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 113 <LLOQ 15.2 553 169 <LLOQ <LLOQ 84 <LLOQ <LLOQ 196 <LLOQ <LLOQ 550 <LLOQ <LLOQ 25 <LLOQ <LLOQ 491 <LLOQ <LLOQ 577 130 732 1440 3130 437 <LLOQ <LLOQ 141 457 452 <LLOQ 127 68 416 C = CatFish, LM = Large mouth bass, SM = Small mouth bass, RW = River water, and RS = River Sediments. thigh triplicate value was statistically eliminated using Dixon's Q.Test. 2(Number of Fish LLOQ I Number of Fish Analyzed). Only one River Water and one River Sediment sample were collected from each sampling location, 3M Environmer_taLlaboratory Page 5 of 276 ReportE02-0443 Tenn. RiverValley Samples PURPOSE The purpose of this studyis to perform quantitativescreening for PFBS, PFHS, PFOA, FOSA, and PFOS in sport-caught fish, river water, and river sediments from three sampling locations of the Tennessee River near Decatur, Alabama. TEST AND ANALYTICAL REFERENCE SUBSTANCES Table2: Characterizationof the Test and AnalyticalReferenceSubstances. TEST AND ANALYTICAL REFERENCE SUBSTANCE PFHS FOSA PFOA Compound Source StorageConditions FOSA, PPFerHflSuo, rohexanesulfonate aPmeridflueorooctanesulfon- 3M SpecialtyMaterials, Bldg.236-2B-11 Frozen 3M SpecialtyMaterials, Bldg.236-1B-10 Frozen PFOA, Perfluorooctanoate Ammonium 3M SpecialtyMaterials, Bldg.236-1B-10 Frozen 3IdMenLtaifb'_oartaiotonNryumber PhysicalDescription Purity TEST AND ANALYTI REFERENCE SUBST_ TCR-083 White Powder 98.6% TCR-029 Lightyellowwaxy solid Undetermined TCR-123 White Powder 95.0% PFOS Compound PFBS,PotassiumPerfluorobutane PFOS,Potassium Sulfonate Perfluorooctanesulfonate Source StorageConditions WildlifeIntemational Frozen 233M6S-1pBe-c1i0altyMaterialsB, ldg. Frozen 3NMumLabbeorratoryIdentification PhysicaDl escription Purity TCR-359 Whitecrystals 97.3% TCR-129 White Powder Undetermined 3M EnvironmentalLaboratory Page 6 of 276 ReportE02-0443 Tenn. River Valley Samples TEST SYSTEMS Table 3a. Descriptionof FishTissueAnalyzedin this Study Source *Types StorageConditions Location1 Location2 TennesseeRiver Catfish LargeMouthBass SmallMouthBass Frozen Downstreamfromthe3M facility near FoxCreek(rivermile296) Acrosstheriverfromthe3M facility (rivermile301) Location3 Upstreamof the3M facility (rivermile307.5) The fishwere filletedand representativealiquotsof thefilletswere analyzed. Table 3b. Descriptionof RiverWaterAnalyzedin this Study RIVER WATER Source StorageConditions Location1 Location2 TennesseeRiver Chilled(approximatel4y C.) Downstreamfromthe3M facility nearFox Creak(rivermile296) Acrosstheriverfromthe 3M facility (rivermile301) Location3 Upstreamof the 3M facility (rivermile307.5) Table3c. Descriptionof RiverSedimentsAnalyzed in this Study Source StorageConditions Location1 Location2 Location3 TennesseeRiver Chilled(approximatel4y0 C.) Downstreamfromthe 3M facility nearFoxCreek(rivermile296) Acrosstheriverfromthe 3M facility (rivermile301) Upstreamof the3M facility (rivermile307.5) 3M Environmental Laboratory Page 7 of 276 ReportE02-0443 Tenn.RiverValteySamples METHOD SUMMARIES The concentrations of PFBS, PFHS, PFOA, FOSA, and PFOS in Fish Tissue, River Water, and River Sediments were determined by using Solid Phase Extraction (SPE) and High Performance Liquid Chromatography-Electrospray/Mass Spectrometry (HPLC/ES/MS). PREPARATORY METHODS The following tables describe the sample preparation methods for the Fish Tissue, River Water, and River Sediment samples. Data Quality Objectives (DQO) are also given for each sample preparation method. Fish Tissue Sample Preparation Method Table 4a. Fish Tissue Sample Preparation Method STEP FISHTISSUESAMPLEPREPARATI.OMNETHOD 1 Approximatel2y g of FishTissueand 8 mL ofASTM TypeI Waterwarehomogenized. 2 The homogenatewascentrifugedto eliminatethefoam andthenshaken/vortexetdore- suspendthe homogenate. 3 Eachhomogenatewas aliquotedintotriplicatesamples.Thiswas accomplishedby transferring1.0 mLof homogenateto3 separate15 mLcenldfugetubes. Matrixspikes(MS)ware preparedfor everyotherhomogenate.Inthiscase,an addiUonal 4 (4"')1.0 mLof homogenatewastransferredto another15 mLcentrifugetube. The MS's ware spikedwith 100 uL ofa 100 ug/mLspikesolutioncontaininegachof thetest substances. 5 5.0 mLof'_cetonilrilwe asthen addedtothe centrifugetubes.The tubeswerecappedand shakenfor 20 minat 300 rpm. 6 Aftermixing,the sampleswerecentrifugedat 3000 rcffor 10 minutestoclarifythe supematant. 7 The supematanwt asdecantedintonew50 mL centrifugetubesand dilutedwith40 mL of water. WatersC-18T_functional,Sep-Paklg, 6cc SPE columns_ attached70 mL reservoirs wereplacedontovacuummanifoldsand preconditionedin the followingmanner. Approximately10 mLofmethanolwas addedto the columnsandthe vacuumwas applied. 8 Oncemostofthe methanolhad beenpulledthroughA, STMType 1 Water was added(5-10 mL). Whenmostofthiswas pulledthrough,morewaterwas added(5-10mL). Whenthem wasonlya smallamountof waterleftinthe reservoirt,he stopcockwasturnedtostopthe vacuumto thecolumn.The columnsware notallowedto go dry. 9 The supematesfrom step7 ware passedthroughthe preconditionedSPE columns.The aqueouseluentwasnotcollected.The columnswareallowedto dryfor at least3 minutes. 10 The analytesware elutedfromtheSPE columnswith2.0 mL of methanolintoautovials. Seethepreparatiownorksheetfsorotherexactamountst,imes,speedse, tc. 3M EnvironmentLaal boratory Page8 of 276 ReportE02-0443 Tenn.RiverValleySamples Table 4b. Preparation of Extracted Calibration Curves for the Fish Tissue. STEP PREPARATIOONFEXTRACTEDCALIBRATIOCNURVESFORTHEFISHTISSUE ThereweretwoextractedFishTissuecalibrationcurves:LargeMouthBassand CatFish, Rangeflndingexperimentws ere donetodeterminewhichFishTissueshadthe lowest endogenouslevelsof theanalytes.Then,one Large MouthBassand oneCatFishsample containingtheleastamountof endogenoustestsubstanceswereselectedas the matrixto constTuctthe calibrationcurves. The Small MouthBasswas analyzedusingtheLarge Mouth Bass calibrationcurve. The procedurefor preparingthe exlTactedcalibrationcurvesis the same as the FishTissue sample preparation,exceptthe volumeswere scaled-upto providea homogeneousbatch of fishtissuematrix. The differencesare as follows: Approximately10 g of Fish Tissueand 40 mL of ASTM Type 1 Water ware combinedand 1 homogenized. 2 1.0 mL of homogenatewas transferredto the appropriatenumberof tubes. 3 Each tubewas spiked with the predeterminedamountof spike solution. Table 4c. Fish Tissue Analytical Data Quality Objectives. STEP FISHTISSUEANALYTICADL ATAC LJALITOYBJECTIVES 1 Allsamplesware preparedin triplicate.The %RSDshouldbe < 25% Marx spikeswere performedon halfof thefishofeachtypefromeachsamplinglocation. 2 Recoveryshouldbe within_+30%fromexpectedvalues.A totalof 18 matiixspikeswere preparedfor the FishTissuesamples. Water blanks,consistingof analiquotof waterrunthroughthe entiresamplepreparationand extractionprocesswerepreparedwi_ samplesfromeachsamplinglocation.Water blanks 3 containing< LLOQof eachanalyteforthe data setin whichthey wererunwere consideredacceptable. Extractionblanks,consistinogf analiquotof methanorlunthougha preconditionedSPE 4 carlddgew, ere preparedfor eachsamplinglocation.ExtraclJobnlankscontaining< LLOQof each analytefor thedata setin whichtheywererunwereconsideredacceptable. 5 Mid-levelcalibrationcurvepointswareused as CCV's. River Water Sample Preparation Method Table 4d. River Water Sample Preparation Method STEP RIVERWATERSAMI_LEPRi=PARATIOMNETHOD 1 WatersC-18Tri-functionaSl,epPak lg, 6cc SPE columnswith attached70 mL reservoirs were placedontovacuummanifoldsand preconditionedinthe followingmanner. Appro)dmatel1y0 mL of methanolwas addedtothecolumnsand the vacuumwas applied. Once mostof themethanolhadbeenpulledthrough,ASTMType 1 Water wasadded(5-10 mL). When mostof thiswas pulledthrough,morewaterwas added(5-10mL). Whenthere was onlya smallamountofwater leftinthereservoirt,he stopcockwas turnedto stopthe vacuumtothecolumn.The coiumnswere notallowedto go dry. 2 40 mL ofthe RiverWater waspassedthrougha preconditionedSPE column.The columns wereallowedto dryfor at least3 minutes. 3M EnvironmentLaal boratory Page9 of276 ReportE02-0443 Tenn.RiverValleySamples Table 4d. River Water Sample Preparation Method 3 The analyteswere elutedfromthe columnswith 2.0 mL of methanolintoautovials. Table 4e. River Water Sample Data Quality Objectives 1 Water blanks,consistingof an aliquotof water run throughthe entire preparationand extractionprocess,were preparedwith sampleseachday samples wereextracted. Water blanks containing < LLOQof each analytefor the data set in which they were run were consideredacceptable. 2 A non-extractedsolventcalibrationcurve was usedto quantitatethe River Water samples. No extractedCCVswere prepared,a mid-levelcalibrationcurve pointwas used for this purpose. 3 No matrixspikes were preformedduringthe sample preparationofthe River Water samples. River Sediment Sample Preparation Method Table 4f. River Sediment Sample Preparation Method STEP RIVERSEDIMENTSAMPLEPREPARATIOMNETHOD Therewere 3 RiverSedimentsamples,one fromeach samplinglocation. Triplicatesamples plus a matrixspike were preparedfor each location. Initially,sedimentwas transferredto 50 mL cantrifugetubes and cent]_Jgedat 6000 RCFfor 1 20 min. The liquidwas decantedoffandtheremainingsedimenwt as usedfor thesample preparation 2 Approximatel2y0g ofsedimenat nd 35mLof 1%AceUcAcid(aqueousw) ere combinedinto 50mLcentrifugetubes. 3 Marx spikeswere preparedby adding100 uL of 100 ug/mLspikesolutiontothe predetermineMd S tubes. 4 Thetubeswere capped,vortexeda, nd then shakenfor60 minat 300 RPM. 5 They werethencentrifugedat 6000 RCFfor20 minutes. WatersC-18Tri-functionaSl,ep-Paklg, 6ccSPE columnswithattached70 mL reservoirs wereplacedontovacuummanifoldsandpre-conditJoneindthe followingmanner. Approximately10 mLof methanowl as addedto thecolumnsandthevacuumwas applied. 6 Oncemostofthe methanolhadbeenpulledthroughA, STMType 1 Water wasadded (5-10 mL). When mostof thiswas pulledthrough,morewaterwasadded(5-10mL).When there was onlya smallamountofwaterleft inthe reservoirt,he stopcockwasturnedto stopthe vacuumtothe column.The columnswerenotallowedto godry. 7 The aqueoussolutionfsromstep#5 weredecantedfromthesamplesand passedthrough pre-condilJoneSdPE cartridges.The aqueouseluateswere discarded. 20 mLof methanolwasthenaddedto the sedimentsamples.The sampleswerevortexed, 8 shakenfor30 rainat 300 RPM,andthencenbifugedat 6000 RCFfor20 minutes. 9 The methanowl as decanted,passedthroughthe SPE cartridgeandcollected. An additional 4 mLofmethanowl as usedtowashthereservoiar ndthecolumn. 10 The collectedmethanolwas then addedto approximatel2y00mLof ASTMType I Water. 11 Thissolutionwasthen passedthrougha newpreconditioned$PE carlTidgeT. he aqueous eluatewas discarded. 12 The analyteswereelutedfromtheSPE cartridgews ith2.0 mLof methanolintoautovials. 3MEnvironmentLaal boratory Page10of 276 ReporEt 02-0443 TennR. iveVr alleySamples Table4g. RiverSedimentSampleDataQuality Objectives STEP RIVERSEDIMENSTAMPLEDATAQUALJTOYBJECTIVES 1 AllsampleswerepreparedinkiplicateT. he%RSDshouldbes 25% 2 Mvaalutreixss.pikeswareperformedoneachsample.Recoveryshouldbewithin+30%of expected Twolabcontrosl amplesc,onsistinogfspikedwatercarriedthroughtheentireextraction processandanalyzedwiththesamplesw, erepreparedH. owevert,heinformaUownasnot 3 usedbecausethedatasuggesteidtwasimpossibleto recovesr pikedanalytesfromacidified waterwhenriversedimenwt asnotpresent. Waterblanks,consistingofanaliquotofwaterrunthroughtheentirepreparatioannd 4 extrac'dopnrocessw, erepreparedA. cceptablevalueswere< LLOQforthe datasetin whichtheywererun. 5 TheRiverSedimenst ampleswerequantitatedusinga non-extractesdolvenct alibration curve.Mid-leveclalibratiocnurvepointswereusedas CCV's. SAMPLE ANALYSIS The sampleswere analyzedusing HPLC/ES/MS. The analyticalmethod was based on the 3M Environmental Laboratory Method ETS-8-155.1"Analysis of Waste Stream,Water Extracts or Other Systems Using HPLC-Electrospray/MassSpectrometry'. The following table details sample run information, including the sequence and the run start date of each sample. Table 5. SampleAnalysisInformation. Catfish I 2 LargeMouthBass 3 SmallMouthBass 4 RiverWater 5 RiverSediments SL-1 SL-2 SL-3 SL-1 SL-2 SL-3 SL-3 SL-1 SL-2 SL-3 SL-1 SL-2 SL-3 D020629 D020629 D020702 D020626 D020628 D020628 D020628 D020812 D020812 D020812 1021112 1021112 1021112 29 Jun02 29 Jun 02 02 Jul 02 26 Jun02 28 Jun02 28 Jun02 28 Jun02 i 12 Aug 02 12 Aug02 12 Aug 02 12 Nov02 12 Nov02 12 Nov02 3MEnvironmenLtaabl oratory Page11of276 ReporEt 02-0443 TennR. iveVr alleySamples ANALYTICAL METHOD Sample analysiswas based on ETS-8-155.1 "Analysisof Waste Stream, Water Extracts Or Other Systems Using HPLC-Electrospray/MassSpectrometry". Methanol extracts were analyzed using HPLC/ES/MS in the negative ion mode. PFBS, PFHS, PFOA, FOSA and PFOS levels were evaluated versus calibration standards ranging in concentration from 11000 ng analyte/mL. The target ions were as follows: m/z = 299 (PFBS), m/z = 399 (PFHS), m/z = 413 (PFOA), m/z = 498 (FOSA), and m/z = 499 (PFOS). The analytical method used for analysis is presented below; modifications may be necessary to optimize the method for individual instruments. Analytical Equipment Liquid Chromatograph: Agilent/Hewlett-PackardSeries1100 LiquidChromatographsystem Analytical column:KeystoneBetasiTlM Cls 2x50mm, 51Jmparticlesize Column temperature: 30 C Cycle Time: 9.5 minutes Flow rate: 300pL/min Injection volume: 4 to 201JL Mobile phase components: Solvent A: 2.0 mM ammonium acetate in water Solvent B: HPLC Grade Methanol Solvent Gradient: Time 0.00 0.50 0.80 3.50 5.50 6.50 9.50 %...BB 10 % 10 % 60 % 100 % 100 % 10 % 10 % Mass Spectrometer: AgilenUI-Lewlett-PackarSderies1100 API/Mass SpectrometerDetector Software:AgilentChemStation A.08.03 FragmentorVoltage:m/z 299 = 100V m/z 399 = 120V m/z 413 = 100V m/z 498 = 80V m/z 499 = 140V CapillaryVoltage: 4000 V Gain = 1.0 EMV Mode: ElectrosprayNegative Gas Temperature:350 C DryingGas:8.0 L/rain. NebulizerPressure:30 psig AnalysisType:SingleIonMonitoring(SIM) 3MEnvironmenLtaabl oratory Page12of276 ReporEt02-0443 Tenn.RiveVr alleySamples ANALYTICAL RESULTS Data qualityobjectivesoutlined in the Preparation Methodssectionwere met. Regressions. Quadratic curve fit was applied to calibration standards and sample data to improve quantitation over the concentration range appropriate to the data. All calibration curves had least-square fits of 0.990 or greater. Calibration Standards. Standards ranging in concentrationfrom approximately 1.0 to 1000 ng/mL were used for the calibration curves. The standard curve points had an injection volume of 10 uL. In some instances, the 1.0 ng/mL standard was injected at smaller volumes (1,2, and 5 uL), this was done to extend the low end of the calibration curve. Calibration curves were run before every analytical sequence. Percent deviations of each calibration standard were calculated. High-end curve points that were outside the +_20%criteria of the target concentrationwere excluded from the curve calculations. Low-end curve points that were outside the +20% criteria were included in the curve calculations but excluded from the Lower Limit of Quantitation (LLOQ). Continuing Calibration Verification (CCV). For quantitative determinations, a mid-level matrix calibration check was analyzed at least every ten samples to monitor instrumental drift, with a limit of _+_20d%eviation of the target concentrations. Lower Limit of QuantitaUon (LLOQ). The LLOQ was equal to the lowest standard in the calibration curve, with a level of accuracy within +20%, that demonstrated a response greater than two times the response of analyte in the blank samples. System Suitability. Five system-suitability standards were analyzed before each initial calibration curve to measure the precision of the retention times and peak area. The precision criterion of +5% for the mean area recovery was achieved. Lab Control Spikes (LCS). LCSswere performed for the River Sediments. However, the information was not used because the data suggested it was impossible to recover spiked analytes from acidified water when river sediment was not present. Matrix Spikes (MS). Matrixspikeswere performedfor the FishTissueand the River Sedimentsamples, Desirablematrixspikerecoveriesare 30%, Not allmatrixspikesmet thiscriteria. The FishTissue datawas quantitatedusingan extractedcalibrationcurvewhile the RiverWater and RiverSedimentsampleswere quantitatedusingunextractedcalibrationcurves. The calibrationcurve rangethatwas injectedwas from 1 ng/mLto 1000 ng/mL,butthe rangeused differed. The tablesthatfollowcontaineitherthecalibrationstandardor thesamplepreparation methodLowerLimitof Quantitation(LLOQ)for theanalytesfor each sampleat each location alongwithbatchusedand the analysisdate. The samplepreparationmethodLLOQswillbe annotatedin thetables. 3MEnvironmenLtaabl oratory Page13of276 ReportE02-0443 Tenn. RiverValley Samples Table6a. PFOSCalibrationStandardReprocessinSgummary PFOS CONCENTRATION SAMPLETYPEAND LOCATION Catfish,SL-1 CatfkshS, L-2 Catfish,SL-3 BATCHANDANALYSIDSATE LOWERLIMIT'OF QUANTITATI(OLNLOQ) D020629,29 Jun02 2.5 ng/g D020629,29 Jun02 2.5 ng/g D020702,02 Ju102 1.0 ng/g LargeMouthBass,SL-1 LargeMouthBass,SL-2 D020626,26 Jun02 D020628,28 Jun02 1.0 ng/g 2.5 ng/g LargeMouth Bass,SL-3 D020628,28 Jun02 2.5 ng/g SmallMouthBass,SL-3 130206282,8 Jun02 2.5 ng/g RiverWater,SLol D020812A,12Aug02 125 pg/mL* RiverWater, SL-2 RiverWater, SL-3 D020812A,12 Aug02 D020812A,12 Aug02 125 pg/mL* 125 pg/mL* RiverWater, SL-1 D020812B,12 AUg02 12.5 ng/mL" RiverWater, SL-2 D020812B,12 Aug02 1.25 ng/mL* RiverWater,SL-3 D020812B,12 Aug02 1.25 ng/mL* RiverSedimentS, L-1 RiverSediment,SL-2 10211121, 2 Nov02 10211121, 2 Nov02 250 pg/g* 250 pg/g* RiverSediment,SL-3 10211121, 2 Nov02 250 pg/g* DenotessamplepreparationmethodLLOQ. Method LLOQ= InstrumentLLOQ/MethodConcentration Factor. 3M EnvironmentaLl aboratory Page 14 of 276 Report E02-0443 Tenn. River ValJeySamples Table6b. FOSACalibrationStandardReprocessinSgummary FOSA CONCENTRATION SAMPLE TYPE AND LOCATION Catfish,SL-1 Catfish,SL-2 Catfish,SL-3 LargeMouth Bass,SL-1 Large MouthBass,SL-2 LargeMouth Bass,SL-3 Small MouthBass, SL-3 RiverWater, SL-1 RiverWater, SL-2 RiverWater, SL-3 RiverWater, SL-1 RiverWater,SL-2 RiverWater, SL-3 River,Sediment,SL-1 RiverSediment,SL-2 RiverSediment,SL-3 BATCH ANDANALYSIS DATE D020629,29 Jun02 D0206LxJ2,9 Jun02 D020702,02 Ju102 130206262,6 Jun 02 1:)0206282,8 Jun 02 D020628,28 Jun 02 .| D020628,28 Jun02 D020812A,12 Aug 02 D020812A,12 Aug 02 D020812A,12 Aug 02 m,, D020812B,12 Aug02 D020812B,12 Aug02 DO20812B,12 Aug02 10211121, 2 Nov02 10211121, 2 Nov02 10211121, 2 Nov02 LOWER LIMIT OF QUANTITATION(LLOQ) 2.5 ng/g 2.5 ng/g 2.5 ng/g 5.0 ng/g 5.0 ng/g 5.0 ng/g 5.0 ng/g 25 pg/mL* 25 pg/mL* 25 pg/mL* 1.25ng/mL* 1.25ng/mL* 1.25ng/mL* 50 pg/g* 50 pg/g* 5010g/g* DenotessamplepreparationmethodLLOQ. MethodLLOQ = InstrumentLLOQ/MethodConcentration FaVor. 3M EnvironmentalLaboratorye Page 15 of 276 ReportE02-0443 Tenn. RiverValley Samples Table 6c. PFOA Calibration Standard Reprocessing Summary SAMPLE TYPE AND LOCATION Catfish,SL-I CatfL_hS, L-2 Catfish,SL-3 BATCH ANDANALYSIS DATE D020629,29 Jun02 D020629,29 Jun02 D020702,02 Ju102 LOWER LIMIT OF QUANTITATION(LLOQ) 5.0 ng/g 5.0 ng/g 5.0 ng/g Large MouthBass, SL-1 LargeMouthBass,SL-2 Large MouthBass,SL-3 Small MouthBass,SL-3 RiverWater, SL-1 RiverWater, SL-2 RiverWater, SL-3 D020626,26 Jun02 D020628,28 Jun02 D020628,28 Jun02 D020628,28 Jun02 D020812A,12 Aug02 D020812A,12Aug 02 D020812A,12Aug 02 2.5 ng/g 5.0 ng/g 5.0 ng/g 5.0 ng/g 50 pg/mL* 50 pg/mL* 50 pg/mL* RiverWater,SL-1 RiverWater, SL-2 D020812B,12 Aug02 D020812B,12 Aug02 1.25ng/mL* 1.25ng/mL* RiverWater, SL-3 RiverSediment,SL-1 RiverSediment,SL-2 RiverSedimentS, L-3 D020812B,12 Aug02 10211121, 2 Nov 02 10211121, 2 Nov02 10211121, 2 Nov 02 1.25ng/mL* 250 pg/g* 250 pg/g* 250 pg/g* DenotessamplepreparationmethodLLOQ. MethodLLOQ= InstrumentLLOQ/MethodConcentration Factor. 3M EnvironmentaLl aboratory Page 16 of 276 ReportE02-0443 Tenn.River Valley Samples Table6d. PFHSCalibrationStandardReprocessingSummary PFHS CONCENTRATi ON SAMPLETYPEAND BATCHANDANALYSIDSATE LLOOWWEERRLLIIMMITITOOFF LOCATION BATCH AND ANALYSIS DATE QUANTITAATTIIO(OLNNLOQ) Catfish,SL-1 D020629,29 Jun02 2.5 ng/g Catfish,SL-2 D020629,29 Jun02 2.5 ng/g Catfish,SL-3 D020702,02 Ju102 2.5 ng/g LargeMouthBass,SL-1 LargeMouthBass,SL-2 LargeMouthBass,SL-3 SmallMouthBass,SL-3 RiverWater,SL-1 RiverWater,SL-2 RiverWater,SL-3 D020626,26 Jun02 130206282,8 Jun02 D020628,28 Jun02 I)020628,28 Jun02 D020812A,12 Aug02 D020812A,12 Aug02 D020812A,12 Aug02 1.0 ng/g 1.0 ng/g 1.0 ng/g 1.0 ng/g 25 pg/mL* 25 pg/mL* 25 pg/mL* RiverWater,SL-1 D020812B,12 Aug02 1.25ng/mL* RiverWater, SL-2 RiverWater,SL-3 D020812B,12 Aug02 D020812B,12 Aug02 1.25ng/mL* 1.25ng/mL* RiverSedimentS, L-1 RiverSediment,SL-2 RiverSediment,SL-3 10211121, 2 Nov02 10211121, 2 Nov02 10211121, 2 Nov02 100 pg/g* 100 pg/g* 100 Pg/g* * DenotessamplepreparationmethodLLOQ. Method LLOQ= InstrumentLLOQ/MethodConcentration Factor. 3M EnvironmentalLaboratory Page 17 of 276 ReportE02-0443 | Tenn. River Valley Samples Table 6e. PFBS CalibrationStandard ReprocessingSummary PFBS CONCENTRATION SAMPLETYPEAND LOCATION Catfish,SL-1 BATCHANDANALYSIDSATE LOWERLIMITOF QUANTITATIO(LNLOQ) D020629,29 Jun02 5.0 ng/g Catfish,SL-2 D020629,29 Jun02 5.0 ng/g Catfish,SL-3 D020702,02 Ju102 5.0 ng/g LargeMouthBass,SL-1 LargeMouthBass, SL-2 LargeMouthBass,SL-3 SmallMouthBass, SL-3 RiverWater,SL-1 RiverWater,SL-2 RiverWater,SL-3 D020626,26 Jun 02 D020628,28 Jun 02 D020628,28 Jun02 D020628,28 Jun02 D020812A,12Aug 02 D020812A,12Aug 02 D020812A,12Aug 02 1.0 ng/g 2.5 ng/g 2.5 ng/g 2.5 ng/g 50 pg/mL* 50 pg/mL* 50 pg/mL* RiverWater,SL-1 RiverWater,SL-2 D020812B,12Aug 02 D020812B,12Aug 02 1.25ng/mL* 1.25ng/mL* RiverWater,SL-3 RiverSedimentS, L-1 RiverSediment,SL-2 RiverSediment' SL-3 D020812B,12Aug02 1021112,12Nov 02 10211121, 2Nov 02 10211121, 2Nov 02 1.25ng/mL* 100 pg/g* 100 pg/g* 10010g/g* * Denotessample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor. 3M EnvironmentalLaboratory Page 18 of 276 ReportE02-0443 Tenn. River Valley Samples Blanks. Method blanks, Milli-Q water takenthroughthesolidphase extractionprocess,provideda measureof methodbackground.In thisexperiment,theywere labeled as =WB".One set was preparedfor each location. In the FishTissueportionof the experiment,theywere run withthe Catfishsamples. Acceptablevaluesfor the blankswere less than50% of the LowerLimitOf Quantitation(LLOQ). All methodblanksin thisstudymet this criterion. The FishTissue segmentof the experimentalsocontainedmethodblanksfor the SPE cartridges. These were labeledas "SB"and consistedof methanolthatwas usedto extractpre-conditionedcolumnsthatdidnothave anysampleadded. All of thesemethod blanksmet the previouscriterion. Solventblanks/Methanobl lanks(methanolinjections)provideda measure of instrument contamination.Acceptablesolventblanksmustcontainlevelsof targetanalyteless than 50% of the Lower LimitOf Quantitation(LLOQ). All of the solventblanksin thisstudymet thiscriterionexceptthe following: Note - Solvent Blanks that were before the System Suitabil#yinjections and did not pass the criteda are not recorded below. D020626 extractedsamples0050 (PFBS, PFHS, and PFOA)and 0051 (PFHS). These were causedby carryoverfrom higherlevelstandardcurvepoints. The solventblanks thatwere run after these pointsshowedminimalcarryover. D020628 sample0051 (PFBS, PFHS, and PFOA), 0052 (PFHS), and 0053 (PFHS). This was causedby carryoverfrom the high-levelstandardcurve point. The solventblanks thatwere runafter showedminimalcarryover. D020629 samples0059 (PFHS, PFOA, FOSA, and PFOS), 0060 (PFOS), and 0061 (PFHS, PFOA, and PFOS). Thiswas caused bycarryoverfrom high-levelstandardcurve points. The 0061 MethanolBlankhad a significanltevelof analytesbut thishad noeffect onthe qualityof thedata. The next samplehad trace amountsof analyteand was below the LLOQ for all analytes. Therefore,the 0061 MethanolBlankdidnotinfluencethe sample. The nextsolventblank(0067) had nominalanalyteconcentration. D020702 samples0042 (PFOS), 0059 (PFHSand PFOS), 0060 (PFOS), and 0061 (PFOS). Thiswas causedby carryoverfromthehigh-levelstandardcurve point. The solventblanksthat were runafter showedminimal carryover. D020812(A)samples0016 (PFOA and FOSA) and 0031 (PFOA). These were causedby carryoverfromhigherlevelstandardcurvepointsor systemsuitabilitypoints. The solvent blanksthatwere runafter thesepointsshowedminimalcarryover. Samples0037 (PFOA) and 0039 (PFBS, PFHS, and PFOA) had carry-overfrom samples.Subsequent blanks showedminimalcontamination. 1021112samples012 (PFBS, PFOA, and FOSA), 027 (PFBS, PFOA, and FOSA), 039(FOSA), 066, (PFOA and FOSA), 068 (FOSA), and 071 (FOSA). All of thesecanbe attributedto carryoverfrom high-levelstandardsorsamples. 3M EnvironmentalLaboratory Page 19 of 276 Report E02-0443 Tenn. River Valley Samples DATA SUMMARY Tables 7a, 7b, 7c, and 7d presentthe datafor individualsamples. Table 8 summarizes the average data for sample groups. Representativechromatograms are presented in Attachment C. Tables 7a, 7b, 7c, and 7d display the on-column and corrected concentrations for individual samples. Also included are the average concentrationsfor each set of samples standard deviation, and % Coefficient of Variation, when applicable. The final values reported are corrected for dilution/concentration factors introduced during sample preparation and by injection volume differences. The reported values were not adjusted for Matrix Spike Recoveries. When some of the samples within a group were < LLOQ, the average value for the group was calculated using the reported analytical value for samples > LLOQ and the LLOQ value for samples < LLOQ. The abbreviations are as follows: SL - Sample Location, C - Catfish,LM - Large mouth bass, SM - Small mouth bass, RW - River Water, and RS - River Sediment. 3M EnvironmentalLaborator=y Page 20 of 276 Report E02-0443 Tenn. River Vatley Samples Table 7a. Catfish Analytical Data. 42778 42779 42780 42781 42782 42783 42784 42785 42786 42789 42790 42791 42792 42793 42794 42795 42796 42797 SL-1; C-1-1 SL-1; C-1-2 SL-I. C-1-3 SL-1. C-2-1 SL-1. C-2-2 SL-1. C-2-3 SL-1. C-3-1 SL-I. C-3-2 SL-I. C-3-3 SL-I. C-4-1 SL-1. C-4-2 SL-1. C-4-3 SL-1. C-5-1 SL-I. C-5-2 SL-I. C-5-3 SL-1. C-6-1 SL-1. C-6-2 SL-I. C-6-3 SL-2; C-1-1 SL-2; C-1-2 SL-2. C-1-3 SL-2. C-2-1 SL-2. C-2-2 SL-2. C-2-3 SL-2. C-3-1 SL-2. C-3-2 SL-2. C-3-3 SL-2. C-4-1 SL-2. C-4-2 SL-2. C-4-3 SL-2. C-5-1 SL-2. C-5-2 SL-2. C-5-3 SL-2. C-6-1 SL-2. C-6-2 SL-2. C-6-3 SL-2. C-7-1 SL-2. C-7-2 SL-2. C-7-3 SL-3; C-1-1 SL-3; C-1-2 SL-3. C-1-3 SL-3. C-2-1 SL-3. C-2-2 SL-3. C-2-3 SL-3. C-3-1 SL-3. C-3-2 SL3. C-3-3 SL-3. C-4-1 SL-3. C-4-2 SL-3. C-4-3 SL-3. C-5-1 SL-3. C-5-2 SL-3. C-5-3 SL-3. C-6-1 SL-3. C-6-2 SL-3. C-6-3 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <[.LOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 5.9 5.3 5.2 4.4 4.2 3.9 7.0 7.1 7.4 3.9 3.7 3.8 9.1 9.1 8.8 7.0 6.9 7.0 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLCK_ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 58.7 53.5 52.0 44.5 41.7 39.1 70.5 70.8 73.8 39.3 36.7 38.2 91.0 90.7 87.5 69.8 69.1 69.8 54.7 3.49 6.4% 41.8 2.67 6.4% 71.7 1.85 2.6% 38.1 1.30 3.4% 89.8 1.95 2.2% 69.5 0.41 0.6% 11.2 10.5 10.0 9.8 9.2 8.6 16.1 17.9 19.2 17.1 16.2 16.6 8.1 8.0 7.8 5.9 6.0 5.9 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 1.9 1.9 1.4 1.2 1.1 1.2 <LLOQ <LLOQ ,:LLOQ i 3.7 3.5 4.0 <LLOQ <LLOQ <LLOQ <LLOQ 2.3 2.3 112.1 104.7 100.3 97.6 91.8 86.1 161.2 179.4 192.4 171.5 161.9 165.8 80.8 80.2 77.5 58.8 59.7 58.7 106 6.00 5.7% 91.8 5.77 6.3% 178 15.67 8.8% 166 4.82 2.9% 79.5 1.74 2.2% 59.1 0.57 1.0% 18.8 17 18.7 2.75 14.0 16.0% 11.5 11.7 11.5 0.44 12.2 3.7% 36.9 35.1 40.4 37.4 2.72 7.3% 23.3 23.5 23.2 3M EnvironmentaLl aboratory Page 21 of 276 ReportE02-0443 Tenn. River Valley Samples Table 7b. Large mouth and Small mouth Bass Analytical Data. 42799 42800 42801 42802 42803 42804 42805 42806 42807 42808 42809 42810 42811 42812 42813 42814 42815 SL-1; LM-I-1 SL-1; LM-1-2 SL-1. LM-1-3 SL-1. LM-2-1 SL-1, LM-2-2 SL-1. LM-2-3 SL-1. LM-3-1 SLol. LM-3-2 SL-I. LM-3-3 SL-1. LM4-1 SL-I. LM-4-2 SL-I. LM4-3 SL-I. LM-5-1 SL-I. LM-5-2 SL-I. LM-5-3 SL-1. LM-6-1 SL-I. LM-6-2 SL-I. LM-6-3 SL-2; LM-I-1 SL-2; LM-1-2 SL-2. LM-1-3 SL-2. LMo2-1 SL-2. LM-2-2 SL-2. LM-2-3 i SL-2. LM-3-1 SL-2. LM3-2 SL-2. LM-3-3 SL-2. LM-4-1 SL-2. LM-4-2 SL-2. LM-4-3 SL-3; LM-I-1 SL-3; LM-1-2 SL-3. LM-1-3 SL-3. LM-2-1 SL-3. LM-2-2 SL-3. LM-2-3 SL-3. LM-3-1 SL-3. LM-3-2 SL-3. LM-3-3 SL-3. LM-4-1 SL-3. LM-4-2 SL-3. LM-4-3 SL-3. LM-5-1 SL-3. LM-5-2 SL-3. LM-5-3 SL-3. LM-6-1 SL-3. LM-6-2 SL-3. LM-6-3 SL3. LM-7-1 SL-3. LM-7-2 SL-3. LM-7-3 SL-3. SM-I-1 SL-3. SM-1-2 SL-3. SM-1-3 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ,,, <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 6.4 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 64.3 (Eliminated via Q-Testt <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 18.5 13,0 14.0 63.6 61.4 57.2 73.2 80.8 82.4 68.8 75.7 65.3 46.6 41.5 38.9 69.3 59.9 66.0 <LLOQ <LLOQ <LLOQ 2.6 <LLOQ <LLOQ 9.7 11.8 8.5 53.1 54.1 56.9 <LLOQ "<LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 185.5 130.0 139.7 635.5 614.0 571,7 732.1 807.7 824.4 688.4 757.0 653.3 465.5 415.0 388.7 693.2 599.1 660.2 25.6 i 96.7 117.6 64.7 530.8 540.9 569.4 152 29.61 19,5% 607 32.49 5.4% 788 49.18 6.2% 700 52.70 7.5% 423 39.03 9.2% 651 47.78 7.3% 100 16.68 16.7% 547 20.02 3.7% 3M EnvironmentaLl aboratory Page 22 of 276 ReportE02-0443 | Tenn. River Valley Samples Table 7c. River Water Analytical Data. 38025 38026 38033 38034 38037 3.0 1.50 3.7 1.85 <LLOQ <LLOQ SW02 <LLOQ 38025 38026 38033 38034 <LLOQ <LLOQ 75 84 93 <LLOQ <LLOQ 196 <LLOQ 38025 38026 38033 38034 38037 38038 SW02 21.3 22.7 <LLOQ <LLOQ <LLOQ <LLOQ 10.66 11.33 533 550 566 <LLOQ <LLOQ 38025 38026 38033 38034 38038 1.0 0.48 1.0 0.51 <LLOQ <LLOQ <LLOQ 24 25 26 <LLOQ 38025 38026 38033 38034 38037 38038 SW01 SW01-Dup SW03 SW03-Dup SW02 SW02-Dup 18.5 20.8 <LLOQ <LLOQ <LLOQ <LLOQ 9.25 10.40 462 491 I 520 <LLOQ <LLOQ I The sample extracts were analyzed several times using different sized injection volumes in order to match the appropdate analytical ranges for extracted samples, matrix spikes, and calibration curves. Table 7c incorporates data using 20 uL extracted sample injection volumes, 2 uL ma_ix spike injection volumes, and 10 uL calibration curve injection volumes. 3M EnvironmentaLl aboratory Page 23 of 276 Report E02-0443 Tenn. River Valley Samples Table 7d. RiverSedimentAnalyticalData. LIMS # 38044 38044 38044 38045 38045 38045 38046 38046 38046 38044 38044 38044 38045 38045 38045 38046 38046 38046 38044 38044 38044 38045 38045 36045 38046 38046 38046 LIMS # 38044 38044 38044 38045 38045 38045 38046 38046 38046 38044 38044 38044 38046 38045 38045 36046 38046 38046 Sample Name 38044-1, SL-1 38044-2, SL-1 38044-3, SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 Sample Name 38044-1, SL-I 38044-2, SL-1 38044-3, SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 Sample Name 38044-1, SL-1 38044-2, SL-1 38044-3, SL-1 38045-1, SLo3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 Sample Name 38044-1, SL-1 38044-2, SL-1 38044-3, SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 36046-1, SL-2 38046-2, SL-2 38046-3, SL-2 Sample Name 38044-1, SL-1 38044-2, SL-1 36044-3, SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 On Column PFBS (ng/g) 10.6 10.6 13.5 8.9 8.3 10.0 8.9 8.2 11.7 On Column PFHS (ng/g) 2.7 2.6 2.5 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ On Column PFOA (ng/g) 16.2 14.1 13.7 <LLOQ 2.6 <LLOQ <LLOQ <LLOQ <LLOQ On Column FOSA (ng/g) 29.7 32.4 24.5 1.2 1.2 1.7 2.9 2.5 3.2 On Column PFOS (ng/g) 67.7 70.3 50.4 9.1 6.8 9.1 9.0 8.5 10.5 Adjusted for Inj. Vol. (nglg) 5.3 5,3 6.7 4.4 4.1 5.0 4.5 3.1 5.8 Adjusted for Inj. Vol. (ng/g) 1.4 1.3 1.2 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ Adjusted for Inj. Vol. (ng/g) 8.1 7.1 6.9 <LLOQ 1.3 <LLOQ <LLOQ <LLOQ <LLOQ Adjusted for Inj. Vol. (ng/g) 14.8 16.2 12.2 0.6 0.6 0.8 1.5 1.3 1.6 Ad iusted for Inj. Vol. (ng/g) 33.8 35.1 25.2 4.5 3.4 4.6 4.5 4.2 5.3 Adjusted for Sample Prep. (pg/g) 530 530 674 444 415 502 447 309 583 Adjusted for Sample Prep. (pg/g) 136 132 124 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ , Adjusted for Sample Prep. (pg/g) 810 705 666 <LLOQ 131 <LLOQ <LLOQ <LLOQ <LLOQ Adjusted for Sample Prep. (pg/g) 1484 1618 1223 62 60 83 146 126 161 Adjusted f(_r Sample Prep. (pg/g) 3383 3513 2518 454 342 456 462 425 526 Average, Std. Dev., and %C.V. (pglg) 577 84 14% 452 44 10% 437 137 31% Average, Std. Dev., and %C.V. (pg/g) 130 6 5% <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ Average, Std. Dev., and %C.V. (pglg) 732 67 9% 131 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ Average, Std. Dev., and %C.V. (pg/g) 1439 201 14% 68 12 18% 141 17 12% Average, Std. Dev., and %C.V. (pg/g) 3132 541 17% 416 65 16% 457 52 11% Summaries for theaverage analyteconcentrationper samplinggroupand locationare given below. 3M EnvironmentaLl aboratory Page 24 of 276 Report E02-0443 Tenn, River Valley Samples Table 8. SampleLocation,SampleType,and AnalyticalData Summary. Sampling Location & SpeciesSampled <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ1 <LLOQ <LLOQ <LLOQ 60.9 (6/6)2 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 113 <LLOQ 15.2 553 169 i <LLOQ <LLOQ 84 <LLOQ <LLOQ 196 <LLOQ <LLOQ 550 <LLOQ <LLOQ 25 <LLOQ <LLOQ 491 <LLOQ <LLOQ 577 130 732 1440 3130 437 <LLOQ <LLOQ 141 457 452 <LLOQ 127 68 416 C = CatFish, LM .=Large mouth bass, SM = Small mouth bass, RW = River water, and RS = River Sediments. 1Hightriplicate value was statistically eliminated using Dixon's Q-Test. 2(Number of Fish > LLOQ I Number of Fish Analyzed). Only one RiverWater and one River Sediment sample were collected from each samplin_ location. AttachmentBcontains additionaldatasummarytables. STATISTICAL METHODS Statisticalmethodswere limitedto calculating averages,standard deviations,% coefficientof variation and statistical examination of outlyingdata points using Dixon's Q-Test. 3M Environmer_taLlaboratory. Page 25 of 276 ReportE02-0443 I I Tenn. River Valley Samples STATEMENT OF CONCLUSION Fish Tissue: FishtissueobtainedfromSample Location1 containedquantifiablelevelsof FOSA and PFOS. Fishtissueobtainedfrom SampleLocations2 and 3 containedquantifiablelevelsof PFOS onty. River Water: Water fromSamplingLocation1 containedquantifiablelevelsof PFBS, PFHS, PFOA, FOSA, and PFOS. Water obtainedfromsample Locations2 and 3 didnotcontainquantifiablelevelsof analytes. River Sediments: River Sedimentobtainedat SampleLocation1 containedquantifiablelevels of PFBS, PFHS, PFOA, FOSA,and PFOS. RiverSedimentobtainedat sampleLocation2 containedquantifiable levelsof PFBS, FOSA, and PFOS. RiverSedimentobtainedat sampleLocation3 contained quantifiablelevelsof PFBS, PFOA, FOSA,and PFOS. REFERENCES 1. 3M EnvironmentaMl ethodETS-8-155.1 "Analysisof Waste Stream,Water ExtractsOr Other SystemsUsingHPLC-Electrospray/MasSspectrometry'. LIST OF ATI'ACHMENTS AttachmentA: AnalyticalMethodand SOP Deviations AttachmentB: Data SummaryTables AttachmentC: SampleChromatograms AttachmentD: Sample PrepSheets,Test Substance,and Test SystemInformation AttachmentE: Notesto File REPORT REVISIONS Typographicael rrorsfor theunitdesignatorsforTables 1, 6a-e, 7a, 7b, 7d, and 8 were corrected. The numberof fish sampledat each locationwas alsoaddedto Tables 1 and 8. The descriptions of the samplinglocationswere adjustedin the summaryand intables 3a, 3b, and 3c to reflect thosereportedin theEntrixreport,July,2003 (project#178401). Removedtwovaluesfor PFHS in riverwaterin tables 1 and 8 becausetheywere <LLOQ. Re-calculatedaveragevaluesfor PFOS in fishat samplinglocations2 and 3 and PFOA in sedimentat samplinglocation3 in tables 1 and 8 usingLLOQ valuesforsamples< LLOQ. 3M Environmental Laboratory Page 26 of 276 Report E02-0443 Tenn. RiverValley Samples SIGNATURE PAGE We certifythat thisreportis a trueand completerepresentationof the datafor thisstudy: _S;taurDd_iryeEct.o_r =,efso--_-_/ - Date'/ /- WilliamK. Reagen, TestingFacilityManagement Date 3M Environmental Laboratory Page 27 of 276 Report E02-0443 II I I Tenn. River Valley Samples ATTACHMENT A: ANALYTICAL METHOD AND SOP DEVIATIONS 3M Environmental Laboratory Page 28 of 276 ReportE02-0443 Tenn.RiverValleySamples Document may be used, if current, for 14 days from 3M ENVIRONMENTALLABORATORY 11/21/2002 METHOD ANALYSIS OF WASTE STREAM, WATER EXTRACTS OR OTHER SYSTEMS USING HPLC-ELECTROSPRA/MAss SPECTROMETRY Method Number:. ETS-8-155.1 Author: Mark L. Anderson,Mark E. Ellefson Approved By: Adoption Date: |J //_ [ 0o Revision Date: _'[3o[o_ Laboratory-lVIarmg=" Orott_Le_et" "_ t...-- /e _ - Dam -' 3MEnvironmentLaal boratory Page29 of276 Report E02-0443 Tenn. RiverValley Samples ._ Document may be used, if current, for 14 days from 11/21/2002 1.0 SCOPE AND APPLICATION 1.1 Scope: This method describes the analysisof waste stream, watersamples or other systems using HPLC-electrospray/massspectrometry. 1.1.1 Specific analytes, ions, matrices, solvents, solutions, quality controls, internal standard(s)andother parameterswill be defined in the protocol or the sample preparationworksheet(s). 1.2 Applicable Compounds: Electrosprayionizable compounds. 1.3 Matrices: 1.3.1 Waste Streamsandothersystemsmay consist of aqueousand/or organicsolvent systems or as designatedin the protocol or sample preparationworksheet(s). 1.3.2 Water Samples include tap water, ground water,wastewaterand other aqueous solutions. The matrixwill be defined by the protocolor sample preparation worksheet(s). 2.0 SUMMARYOrMSTHOD 2.1 This method describesthe analysisof electrosprayionizablecompounds,using HPLCelectrospraymass spectrometry(HPLC-ES/MS). Theanalysisis performedby the mass selection of a single ion characteristicof a particularcompound. 3.0 DEFINITIONS 3.1 Atmospheric Pressure Ionization (API): CommerciallyavailableHPLC-ES/MSsingle quadrupolesystems allow forvariousmethods of ionizationby utilizing a variety of sourcepsr,obes, andinterfaces, Theseincludbeutarenotlimited to:Electrospray Ionizati(oEnSI)A,tmospherPircessurcehemicaIlonizati(oAnPcl)T,hermos'preatyc,. The ionizationtnhesperocessoecscurastatmospherpircessu(rie.en.o,tundera vacuum). 3.2 Electrospray Ionization (ES, ESI): A method of ionizaiionperformedat atmospheric pressure,wherebyions in solutionaretransferredto the gasphase via tiny charged droplets.These dropletsareproducedby the applicationof a strong electricalfield. 3.3 Mass Spectrometer (MS): CommerciallymanufacturedMS systemsareequipped with singlqeuadrupomlaessselectidveetectorIso.nsareselectoendthebasiosfmassto chargreati(om/z)andsubsequendteltyected. 3.4 MicromassMassLynx/HP ChemStafioSnoftwareS:ystemsoftwardesignefdorthe specifoipceratioofnanHPLC-ES/MS.Pleasreefetrothemanualforthespecific instrumesnotftware. 3M EnvironmentaLlaboratory ETS-8-1$$. i AnalysisUsingHlPLC-Eiectrospmy/MSmpsectrometry 3M EnvironmentalLaboratory Page2 of 10 Page 30 of 276 Report E02-0443 Tenn. RiverValley Samples Document may be used, if current, for 14 days from 11/21/2002 4.0 W/d_NINGS AND CAUTIONS 4.1 Health and Safety Warnings: 4.1.1 Use cautionwith the voltagecables forthe elvctrosprayprobe. Whenengaged, the probeemploys a voltageof approximately5000 Volts. 4.1.2 When handling samples or solvents wear appropriate protective clothing, gloves, and eyewear. 4.2 Cautions: 4.2.1 Operatesolventpumps below a backpressurof 400 bar (5800 psi). If the baclcpressureexceeds 400 bar, the HP1100 will initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness. 5.0 INTERFERENCES 5.1 To minimize interferenceswhen analyzingsamples, Teflon should not be used for sample storage or any part of instrumentationthat comes in contact with the sample or extract. 6.0 EQt_PMENT 6.1 Equipmentlisted below may be modifiedin orderto optimize the system. Documentany modificationsin the rawdata as methoddeviations. 6.1.1 MicrornassPlatformLCZMass Spectrometer(orequivalent)equippedwith an electrosprayionizationsource. 6.1.2 HP1100 low pulse solventpump,solvent degasser,column compartment,and autosampleror equivalentHPLCsystem. 7.0 StrrPLn_s AND MA'rERIALS 7.1 Supplies 7.1.1 High pm-itygradenitrogengas regulatedto approximately100 psi (orhouse air system.). 7.1.2 HPLCanalytical column,such as a Betasil CI8 column (50x2mm, 5 _ particle size) or equivalent. 7.1.3 Capped autovials or capped 15ml.,centrifuge tubes. 8.0 REACENTSANDSTAND_,RVS 8.1 Reagents: 8.1.1 Methanol,HPLCgradeor equivalent. 3M EnvironmentaLlaboratory ETS-II-155.1 AnalysisUsingHPLC.Eitrospray/MSmpsectrometry Page3 of 10 3M EnvironmentalLaboratory Page 31 of 276 Report E02-0443 Tenn. RiverValley Samples Document may be used, if current, for 14 days from 11/21/2002 8.1.2 Milli-Q TM water (ASTM type I), all water used in this method should be Milli-Q TM water or equivalent, and may be provided by a Milli-Q TOC Plus system or another vendor. 8.13 Ammonium acetate, reagent grade or equivalent. 8.1.3.1 When preparing different amounts than those listed, adjust accordingly. 8.1.3.2 2.0 mM ammonium acetate solution: Weigh approximately 0.300 g ammonium acetate. Pour into a 2000 L volumetric flask, add the appropriate volume of Milli-Q water, mix until all solids are dissolved. Store at room temperature. 8.1.4 Other solventsand solutionsmay be used asstatedin the protocol or the sample preparationworksheet. 8.2 Calibration Standards: 8.2.1 Typically two method blanks (Milli-Q water), two matrix blanks, and a minimum of5solvensttandardasreanalyzewditheachgroupofsamples. 9.0 SXMrLV.HANDLING 9.1 Standards and prepared samples may be stored in capped autovials, capped 15 mL centrifuge tubesorother suitable containers until analysis. 9.2 If analysis will be delayed, standards and prepared samples may be refrigerated at approximately 4* C until analyses can be performed (refrigerator temperatures may have a detrimental affect on the solubility of saturated solutions). 10.0 Qu_aaTY CONa_OL 10.1 Blanks: 10.1.1 Solvent blanks, method blanks, and matrix blanks are prepared and analyzed with each sample set to determine contamination or carryover. 10.1.1.1 When the study matrices consist of highly purified solvents such as Type 1 water or HPLC grade organic solvents, the method and matrix blanks may be represented by a single solvent blank. 10.1.2 Solvent blanks should be analyzed prior to each calibration curve. Method blanks and matrix blanks should be analyzed after the initial calibration curve but prior to the study samples. If can'yovcr is a problem, consecutive solvent blanks may be necessary. 10.2 Matrix Spikes: 10.2.1Matrixspikesmay bepreparefdoreachsetofextractesdamples(ifapplicablteo thestudy)andanalyzetdodetermineextractieofnficiency. 3MEnvironmentaLlaboratory ETS-8-155I. AnalysisUsingHPLC.ElcfArospray/MSapsesctrometry Page4 of 10 3M EnvironmentalLaboratory Page 32 of 276 Report E02-0443 I I |I I Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 10.2.2 Matrix spike duplicates may be prepared periodically to measure the precision associated with the analysis. 10.2.3 Analyze the matrix spike and matrix spike duplicate (if prepared) in the same run as the original sample. 10.2.4 Matrix spike and matrix spike duplicate concentrations should fall in the mid- range of the initial calibration curve or should be prepared at 1.5-5 times the endogenous concentration of the analyte. Spike concentrations should fall in the low-rangoef theiniticaallibraticounrveif extremellyowlevelasreexpected. 10.3 Continuing Calibration Verifications: 10.3.1 Continuing calibration verifications (CCV) are analyzed to verify the continued accuracyofthecalibraticounrve. 10.3.2Analyzeamid-rangecalibratisotnandaradfteerverytenthsample,witha minimum of one per sample set. 10.4 Internal Standard/Surrogate Standard: 10.4.1 An internal standard (IS) may be used to quantify the target avalytes by establishing a relationship between the ratio of analyte response to IS response and a known concentration of the analyte of interest. The IS should be spiked at an amount that will fall within the mid-range of the calibration curve. The IS shouldbeaddedaftetrheextractipornocessandbeforeanalysis. 10.4.2A surrogatsetandarmday beusedforqualitcyontrolT.he surrogatiesusedto quantitativeevlayluatteheentiraenalyticparloceduriencludinsgample preparatiaonndanalysisT.he surrogatsehouldbespikedatthebeginninogfthe samplepreparatiaonndshouldfalwlithinthelowtomid-rangoef_e calibration curve. 11.0 CALIBRATION AND STANDARDIZATION II.I Analyzethestandarcdurvespriotroandfollowinegachsetofsamples.The averageof two standarcdurvesmay beplottebdylinearregressi(oyn=mx +b) weightedI/x,or quadratifcit(y_ ax2+ bx + c)usingMassLynxorothersuitablseoRware,The calibraticounrvesshouldnotbeforcetdhroughzero. 11.1.1The closincgalibraticounrvemay beexcludediftheCCV's meetacceptable criteriaI.fonlythefirscturveisused,thecalibratiaonndstandardization pararaeters are the same. 11.2 I.fthe initial calibration curve does not meet acceptance criteria perform routine maintenance or prepare a new standard curve (if necessary) and reanalyze. 11.3 For purposes of accuracy when quantitating low levels ofanalyte, it may be necessary to use the low end of the calibration curve rather than the full range, Example: when 3M Enviromnental laboratory ETS-g-155.1 Analysis Using HPLC-Elecu_spray/Mass Specuometry Page 5 oflO 3M Environmental Laboratory Page 33 of 276 Report E02-IM43 I II Tenn. River Valley Samples -.. Document may be used, if current, for 14 days from 11/21/2002 attempting to quantitate approximately 10 ppb of analyte, generate a calibration curve consisting of the standards from 5 ppb to 100 ppb rather than the full range of the curve (5 ppb to 1000 ppb). This will reduce inaccuracy attributed to linear regression weighting of high concentration standards. 11.4 High and/or low points may be excluded from the calibration curves to provide a better fit over the linear range appropriate to the data or because they did not meet the predetermined acceptance criteria. Low-level curve points should also be excluded if their area counts are not at least twice that of the method blanks. Justification for exclusion of calibration curve points will be noted in the raw data. 11.4.1 A minimum of 5 points will be used to construct the calibration curve. 12.0 PROCEDUR_ 12.1 Acquisition set-u p- please reference the SOP that pertains to the specific instrument. Actual parameters will be recorded on the instrument printouts. 12.1.1 Set up the sample list. 12.1.1.1 Assign a sample list filenarne using the first letter of the name of the instrument (T for Tucker), the year (00 for 2000), the month (04 for April), and the day (T001012 for October 12, 2000 on Tucker). If more than one list is made on the same day, use increasing letters of the alphabet starting with A at the end of the list. 12.1.1.2 12.1.1.3 12.1.1.4 Assign a method (MS) file. Assign an HPLC program (Inlet file). Type in sample descriptions and vial position numbers. 12.1.2 To create a method, click on method in the Acquisition control panel then mass spectrometer headings and select SIR. Set ionization mode as appropriate and mass to 499 or other appropriate masses. A full scan is usually collected in addition to the SIRs. Save acquisition method. See the Mieromass MassLynx GUIDE TO DATA ACQUISITION for additional information. 12.1.3 Typically the analytical batch run sequence begins and ends with a set of solvent standards. 12.1.4 Samples are analyzed with a continuing calibration verification (CCV')"injected after every tenth sample. Solvent blanks should be analyzed periodically to monitor for possible analyte carryover. 12.2 Using the AutosamplerlColumn Heater 12.2.1 Place sample vials into the sample tray according to the sample list prepared in Section 12.1.1. 3M Envkonmental Laboratory ETS-8-155.1 Analysis Ustnlg HPLC-Electrmpray/M=mSpectrometry Page 6 of 10 3M Environmental Laboratory Page 34 of 276 Report E02-0443 III __ Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 12.2.2 Attach the proper analytical column in the column heater compartment. If using the switching valve, ensure that the tubing is run to the appropriate ports. 12.3 Using the Inlet Editor 12.3.1 Set-up the HP1100 using the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.3.1.1 Sample size = 10 _tL injection 12.3.1.2 Flowrat = 300 ltL/min. 12.3.1.3 Cyde time = 10.0 minutes 12.3.1.4 Mobile phase components: SolventA:2.0mM Ammonium AcetateinWater SolventB: Methanol(MeOH) Solvent Gradient: Time (rain.) 0.00 1.00 4.50 8.00 8.50 %___BB 5.00 % 5.00 % 95.0 % 95.0 % 5.00 % 10.0 Stop 12.4 Instrument Set-up 12.4.1 Refer to the Platform LCZ User's Guide, the MassLynx NT User's Guide, the ETS-9-36, "Operation and Maintenance of the Mieromass Platform LCZ Eleetrospray/Mass Spectrometer", or the SOP that pertains to the specific ins_m_ent 12.4.2 Check the solvent level in reservoirsand refill if necessary. 12.4.3 Cheek the tip of the stainless steel capillary at the end of the probe with an eyepiece. The tip should be fiat with no jagged edges. If the tip is found to be unsatisfactory, disassemble the probe and replace the stainless steel capillary. 12.4.4 Turn on the nebulizing gas. 12.4.S Open the tune page. Click on 'Operate' to initiate the desolvation heaters. 12.4.6 Open the Inlet Editor. 12.4.6.1 12.4.6.2 Set HPLC pump to "On". Set the solvent flow to the desired flow rate. 12A.6.3 Observe droplets coming out of the tip of the probe. A fine mist should be expelled with no nebulizing gas leaking around the tip of the probe. Readjust the tip of the probe if no mist is observed. 3M Environmental Laboratory ETS-8-155.1 Analysh Us[ag HPLC-Elert,mspm/Mess Spectrometry Pege 7 oflO 3M Environmental Laboratory Page 35 of 276 Report E02-0443 ! I! Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 12.4.6.4 Allow to equilibrate for at least 10 minutes. 12.4.7 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response. Actual parameters will be recorded on the instrument printouts. 12.4.7,1 Drying gas 250-425 liters/hour 12.4.7.2 ESI nebulizing gas 10-15 liters/hour 12.4.7.3 12.4.7.4 12.4.7.5 HPLC constant flow mode, flow rate 10 - 500 I_L/min Pressure <400 bar CIlais parameter is not set, it is a guide to ensure the I-IPLC is operating correctly.) Source Block temperature 150". 12.4.7.6 Desolvafion temperature 250*. 12.4.8 Print the tune page with its parameters, the Inlet page, sample list, mass spectrometer information, and all other applicable information and store it in the study binder with copies taped into the instrument run logbook. 12.4.8.1 All copies must be initialed and dated. 12.4.9 Click on start button on the MassLynx toolbar. Ensure beginning and ending sample numbers encompass all samples to be analyzed. 13.0 DATAANALYSISANDC_TIONS 13.1 Calculations (including, but not limited to): 13.1.1 Calculate matrix spike percent recoveries using the following equation: % Recovery = Observed Result - Background Result x 100 Expected Result 13.1.2 Calculate percent difference using the following equation: % Difference -- Expected Cone. - Calculated Cone. x 100 Expected Cone. 13.1.3 Calculate actual concentration of analyte in matrix (}xg/mL): On-Column Concentration (I.tg/mL) x Dilution Factors = Calculated Concentration 14.0 METHODPERFORMANCE 14.1 The Limit of Quantitation (LOQ) is method, analyte, and matrix specific. For many analytes, the LOQ concentration is selected as the lowest acceptable non-zero standard in the calibration curve. 3M EnvironmentaLlaboratory ETS-S-155.1 AnalysiUssln8 l-IPl_-ElecuosprsyfSlpvclcatrsosncuy Pagc8 of 10 354 Environmental Laboratory Page 36 of 276 ReporEt 02-0443 I j Tenn.RiverValleySamples Document may be used, if current, for 14 days from 11/21/2002 14.2 Solvent and method blank area counts must be < that of the lowest standard used in the calibration curve. 14.3 The coefficient of determination (r2)value for the calibration curve must be greater than or equal to 0.980. 14.4 Continuing Calibration Verification (CCV) percent recoveries must be + 30% of the standard concentration. 14.5 Internal Standard recoveries should be within + 50% of the spiked concentration. 14.6 If criteria listed in this method performance section are not met, maintenance may be performed on the system and samplesreanalyzed or other actions as determined by the analyst. Document all actions in the raw data. 14.7 If data is to be reported when performance criteria have not been met, the data must be footnoted on tables and discussed inthe text of the report. 15.0 POLLUTION PREVENTION AND WASTg MANAGEMENT 15.1 Sample extract waste and flammablesolvent is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers located in the laboratory. 16.0 RECORDS 16.1 Each page generatedfor a study must have the following information included eithcr in the header or hand written on the page: study or project number, acquisition method, integration method, sample name, extraction date, dilution factor (if applicable), and analyst. 16.2 Print the tune page, sample list, acquisition method and all other applicable information to include in the appropriate study folder. Copy these pages and tape into the instrument run logbook. 16,3 Plot the calibration curve then print these graphs and store in the study folder. 16.4 Print data integration summary, integration method, and chromatograms andfile in the study binder. 16.5 Summarize data using suitable softwareand storein the study binder. 16.6 Back-up electronic datato appropriatemedium. Recordthe file names and location of backed-up electronicdatain the studybinder. 16.7 Documentation ofanalyte(s) and all reference substanceswill include mace numbers, lot #'s, purity, expiration, and storage conditions. 17.0 ATTACHMENTS 17.1 None 3MEnvironmenLtaalboratory ETS-8-155.1 AnalysiUs singHPLC-Elcctrospray/SMpaescstrometry Page9 of 10 3M EnvironmentLaal boratory Page37 of276  ReporEt02-0443 II .... TennR. iveVr alleySamples Document may be used, if current, for 14 days from 11/21/2002 18.0 REFERENCES 18.1 Platform LCZ User's Guide, Micromass UK Limited, Tudor Road, Altrincham, WA 14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.2 MassLynx NT User's Guide, Mieromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.3 MassLynx NT Guide To Data Acquisition, Mieromass UK Limited, Tudor Road, Altrincham, WAI4 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.4 ETS-9-34.0, "Operation and Maintenance of Hewlett Packard I-IPLC 1100 System Equipped with a Mass Spectrometer Detector and/or a Photo Diode Array Detector". 18.5 ETS-9-36.0, "Operation and Maintenance of the Micromass Platform LCZ Eleetrospmy//Vlass Spectrometer". 19.0 AFFECTEDDOCUMENTS 19.1 None 20.0 I_VaSIONS Revision Number Reason For Revision Revision Dat_.._.ce 1 TitleChange 09 May0l Section1: Enlargedthescopeof themethodbyincludingadditionaml atrices.Alsoadded commentsaboutspecificparameterwsill bedefinedintheprotocolorprepsheets. SectionsI and2: Removedreferencestospecificcompounds. Section3: RemovedparagrapohnConventionavls. Z-Sprayprobeinterface. Section3: Changedtoallowdifferentsystemsandsoftware. Segtton It: Added paragj'aph allowin S for the use of alternative solvents and solutions. Section9: Broadenetdhetypesof storagecontainersandconditions. Section10: Addedcommentstoallowforflexibilityinqualitycontrolsfordifferentypesof studiaensdapplicability. Section1h Addedaparagrapahllowingforthe excludingof the secondcurve. Section11: Addeda paragrap(hI1.4)allowingforthedroppingofcurvepointsandminimum numberof curvepointsneeded. Section12: AddedcommentstoreferencethespecificSOP'sforset-up. Section12: Correctednumbering. Section16: Addedparagrapohnrecordsof analytesandsubstances. Section18: Addedreferenceto themethodfortheHewlett-PackarLdC/MS. 3M Environmental Laboratory ETS-8-155.1 Analysis Using HPLC-Electmspray/Mms Spectrometry 3M Environmental Laboratory Page 10 of 10 Page 38 of 276 IIII ==1 Report E02-0443 Record of Deviation L Identification Tenn.River Valley Samples Study / Project No. Deviation Type: (Check one) TN River VaUeyE02-0443 [] SOP [] Protocol _Method [] EquiPment Procedure [] Other: Document Numberi ETS'4-04.0 ......... Date(s) of occurrence: .... II. Description: Required Pr0cedure/process;.._..ETS,4-04.0 sectio n 4 states.,.,It is..the responsibility of anyone handling samples to record the movement of those samples on the internal chain of custody form." " ....................................... Actual Procedure/process: The internal chain of custody forms were not generated or used in th e course of this study. ........... IlL Actions Taken: ............................................(.s..u..c..h...a..s...a..m...e..n..dment .issued, SOP revision., etc.)......................................................... Noaddi.tiona! acfionw!.U_.betaken, as_the information..cannot be recalled so !ong after _e. fact..... Recorded By: .................. :t_ ( t ,; ] IV. Impact on Study / Project Thisdeviation does n0tadverseiy a(fect tlae quality of the datal i... Date: ........................... _,,_c ()Z "............ . .i "._ / Authorized By: (StudyJgirctor/.P.roiect Lead) .... -,, ,, y," / ,' _."_ .. 3)' .. ,/ . /"-" . .,..-_--_- / Date: ..,,/, 3M Environmental Laboratory Deviation No. / (assigned by Study Director or Project [.e'Mat theend of study or project) 3M EnvironmentalL_boratory Page 39 of 276 Report E02-0443 ATTACHMENT B: DATA SUMMARY TABLES . _ Tenn. RiverValley Samples 3M Environmental Laboratory Page 40 of 276 Report E02-0443 - - Tenn. River Valley Samples ReportE02-0443 Tenn. 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" _ ++:_,_,.,,,.,._..,._I,.>.................................. <....< <'<<.... <:<:<':"<:<'<<'<<: <" ; _: : : :: 3:; !: : : _: : : : : : ) :: _ : !: ; : :! Report E02-0443 - - Tenn. River Valley Samples Report E02-0443 !=t i# ! i i -i _i_ =_ =1 !:_- i, =i :i :i i_i:t +_8;,_8.8_=8.:8=o8..8.:._888 Ii i i jii i# !# i# i i i i =_i=e I p. i" i" i i i '_= = = i _j : = 1_. I I ' I ii ! t ,_,,.;;,:_tJ_ =._, ,=._.:_ .,=:_.- .=. o:,.,_ o :==3,-:-8_ o o P_ +!-+ii,,i - N , 8 888.818818=1 88 I1 I| I=1 Ill il I! = Ill lOlll =[ mO;ml I ,It .i I _ = ' ti IIi I II ,.; __1 _=__ i'i !" I i om ._8.J' ,,8,,,_,_8..Jg 8:,,8.___8:,.8.._,=,_88..J8.J i I_- im ; I I :._ oo ,. I fILL_ ,_o . =,' o tIR ,_ oi t,i I_ tu &lli ul,l,,u_,.u_'..lUl I mmm i _.... I :_ _'; "'_ '_ ZI'*Z'TZ' Z_Z; :Z, ZZ2 ="+I "i_ o i_'_I " " * .... ,! _ =:_ :;=.m+_ liw _ =:_I= l_w_ _l+w_=_=+='U,',=l_u=_el l= = ! i-) i ; i I =' ++.=_=+=+.+|,+==+=.-,=== - :o o:o+i oI+oi o +to oI_!o .o I ,i oI = oIi_o oIo+i:o+ o o _=-,I>=-+:_I>:_- :,_I :=>;. ::_- >-:+=>:-=:)- :>.:>=.=>_- := - -l- 'I- -I,- -:- I::_ -I- -:- -l-:- --- I: _uw: wlm U_IILwIII_W_l_ u_._uluItuW,l_+UguJ lu u "- Tenn. River Valley Samples ..+ "_ l ,_  ReportE02-0443 - _ Tenn. RiverValley Samples 1021112 River Sediments SampleLocationst, 2,and3. PFBS (299) In|. Vol Sample Name _mlple Irffo On-Co|unto On-Co|u=nn Gorrtcted Corrlctad for Average Am Amount Average for InJ, Vol Sample Pr_)p.' Stnd%CDVlind (uL) (ng/mL) 20 0443.3_44- I E02-0443.31_44-1; SL-1; 383859 10.6 20 0443-31_44-2 E02-0443-35044-2; SL-1;' A 383606 10.5 20 0443-35044-3 E02-0443.38044-3; SL-1; 482034 13.5 20 0453-38045-1 E02-O443.3_45-1; SL-3; 325254 8.9 20 0453-38045-2 E02-0443.38045-2; SL-3: A 305101 5,3 20 0463.36045-3 E02-O443-38045-3: SL-3; A 384688 10.0 (ng/mL) 11.6 9.1 (ng/mL) 5.-_ 5.3 6.7 4.4 4.1 5.0 (pglmL) 529 529 673 443 413 500 (pcj/m._.) 577 83 14% 452 44 10% 20 0463-3804,6-I E92-O443.38048-1; SL-2; *_ 327360 6.9 5.9 4.5 435 437 20 0463-38045-2 E02-0443.38046-2; SL-2; A 232748 6.2 3,1 302 134 20 0463-38046-3 E02-0443-35046-3; SL-2; A 420079 11.7 5.8 571 31% PFHS (398) 20 0443-38044-1 E02-0443-38044.1; SL-1; 122835 2.7 2.6 1.4 136 130 20 0443-38044-2 E02-O443.36044-2; SL-1; 118901 2.6 1.3 132 6 20 044338044-3 E02-0443-38044-3; SL-I 111724 2.5 20 0453-38045-1 E02-0443.38045-1; SL-3; 13341 BLOQ 20 0453.38045-2 E02-O443.38045,2; SL-3; 11469 BLDQ 20 0453-38045-3 E02-0443.38045-3; SL-3 12125 BLOQ BLOQ 1.2 SLOQ BLOQ BLOQ 124 _.OQ BLOQ BLOQ 5% SLOG BLOQ BLOQ 20 0463-36046-1 E02-0_,43..36046-1; SL-2; d 17353 aLOQ BLOQ BLOQ aLOQ BLOQ 4'.( 20 0463-36045-2 E02-0443.38046.2; SL-2; d 15434 BLOQ BLOC) BLOQ BLOQ 20 0463-38046-3 E02-O443-38046.3; SL-2; _ 25494 BLOQ PFOA (413) BLOQ BLQQ t_LOQ 2z0_ 004443-,3.60.4_4-.16,,-E_202.-004443,-3_80-434-18; 0S,L-- 21;I:=22-9b5015090:031 16.2 14.1 14.7 8.1 7.1 ., 20 0443-38044-3 E02-0443.38044-3; SL-I_ 253343 13.7 6.9 805 732 704 80 085 9% ::_ 20 0463-38045-I _"4"_._3_04"-_';-_;'_l _',48" B'_'Q '-_" B_O'Q B'_OQ "_'1" 20 0453.31J045-2 E02-0443.38045-2; SL-3; p 60231 2.6 %3 131 BLOQ 20 0453-38045-3 E02-0443.38045-3: SL-.3;..p., 54998 BLOQ BLOQ BLOQ BLOQ 20 0463-36046-2 602-0443.35046-2: SL-2; _ 35197 BLOQ 20 0463.38046-3 E02-0443.35046-3; SL-2; _, 40917 BLOQ FOSA (498) 20 0443.36044-1 603-0443-38044-1; $L-1; _ 1250415 29,7 20 0443-38044-2 E02-0443.38044-2; SL-1; _11361450 32.4 20 0443-38044-3 .E02_3.380,1_3. ;._S.L-1 ; p..1033.771 24,5 zo o,53-35o4_1e02-0,_,5-1; sL-3;t_,5310 12 20 0453.31_045-2 E02-0443.36045-2; SL-3; p 48172 1.2 28.6 1.4 SLOQ 8LOQ 14.8 16.2 12.2 a.6 0.6 BLOQ BLOQ 1461 1615 1221 62 60 aLOQ BLOQ 1436 200 14% 12 20 0463-36046.1 662-0443-38046-1', SL-_ _ 120457 2,9 2.9 1.5 143 141 .! 20 0463-38046-2 E02-0443-38046-2; SL-2; _1 103503 2.5 20 0463.38046-3 602-0443.38046.3: SL-2; _ 133252 3.2 1.3 124 17 1.6 157 12% _',i_ PFOS (4991 ::'i 20 0443.38044-1 E62-0443.38044-1; SL-1; IA 2785277 67.7 62.8 20 0443.38044-2 EO2-O443-38044-2; SL-1; _12885124 70.3 .z; =0 0,4=_0,_ _E_oz3.0.34640_#.SL_:3.:.p_o3"s so.4 : 20 0453.38045-1 E02-0443-38045-1: SL-3; _1 418454 9.1 8.3 20 0453.38045-2 E02-0443.35045-2; SL-3; F 323943 6.6 33.8 35.1 25.2 4.5 3.4 3377 3506 2514 452 341 3132 540 17_ 416 65 20 0453-35045-3 E._0.2__.0443...3.B0_i .S_3.L-3:_,._42_1.8.5 9.1 4.6 2o o_63-a5046.=102_43-=_045s-1_;-2;p417238 s.o 9.3 45 20 0,463-38046.2 E02-0443-38045-2; SL-2; IA 393650 8.5 4.2 20 o_63-35o45-e3o2-o443.35oS,eL-3-2;p; 47_57 lO.5 5.3 455 4_3 415 514 15% 457 51 11_ Sample 38044 35044.MS 38045 38045-MS 38048 38046-MS W_ (g) 20.0 2001 20.1 20.30 20.4 19.98 Regum"=amp_= =r= _ of_ ten wui0_. (_n-Colunlq Avera_ = Average of trip,tales Cor_c_ed for Inl. VoL = On-Cot/_nount" 0.5 Corseted for Sample Prep = On-Co_ AmOUnt e0.5 * 2 " 1000 Sample Weight (Ave) "2" is the Final Vol of Ihe Extract (mL) 3M EnvironmentalLaboratory Page 53 of 276 E02-0443 ._ Tenn. River Valley Samples I IIIII Combined E02-0443 Large Mouth Bass Data Table LIMS # 42798 42799 42800 42801 42802 42803 42804 42805 42806 42807 42808 42609 42810 42811 42812 42813 42814 42815 PFBS (299)!PFHS (399), Sample Name Amount ng/mL S'L-1;LM-I-1 $L-1; LM-1-2 $L-1. LM.1-3 S1.-1.LM-2-1 SL-1. LM-2-2 SL-1. LM-2-3 S'L-1.LM-3-1 SL-1. LM.3-2 SL-I. LM-3-3 SL-I. LM-4-1 SL-1. LM-4-2 SL-I. LM-4-3 SL-1. LM-5-1 SL-I. LM-5-2 :SL-1. LM-5-3 SL-1. LM-6-1 SL-1. LM-6-2 SL-1. LM-6-3 SL-2; LM-I'-I SL-2; LM-1-2 SL-2. LM-1-3 _SL-2. LM-2-1 SL-2. LM-2-2 SL-2. LM-2-3 SL-2. LM-3--1 SL-2. LM-3-2 SL-2. LM-33 SL2.LM-4-1 SL-2. LM-4-2 SL-2. LM-4-3 SL-3; LM-I"-I SL-3; LM-1-2 SL-3. LM-1-3 SL-3. LM-2-1 SL-3. LM-22 SL-3. LM-2-3 SL-3. LM-3-1 SL-3. LM-3-2 SL-3. LM.3-3 SL-3. LM-4-1 SL-3. LM-4-2 SL-3. LM-4-3 SL-3. LM-5-1 SL-3. LM-5-2 SL-3. LM-5-3 SL-3. LM-6-1 SL-3. LM-6-2 SL-3. LM-6-3 SL-3. LM-7-1 SL-3. LM-7-2 SL-3. LM-7-3 SLY'3S. M-I-1 SL-3. SM-1-2 SL-3. SM-1-3 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOC} BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOC) BLOC) BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ" BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ Amount nglmL ' BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ ' BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ" BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 'BLOQ BLOQ BLOQm,, PFOA (413) Corrected Amount nglmL BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 5.4 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BI OQ BLOQ BLOQ BLOQ BLOQ BL(_Q BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ for Smpl Prep (nglmL) 64.3 -' FOSA (498)1 Amount ng/mL Amount ng/mL BLOQ 18.5 BLOQ 13.0 BLOQ 14.0 BLOQ 63.6 BLOQ 61.4 BLOQ 57.2 "BLOC) 73.2 BLOQ 80.8 BLOQ 82.4 BLOQ 68.8 BLOQ 75.7 BLOC) 65.3 BLOQ - 46.6 BLOQ BLOQ 41.5 38.9 BLOQ 69.3 BLOQ 59.9 BLOQ 66.0 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 2.6 BLOQ BLOQ BLOQ BLOQ 9.7 BLOQ 11.8 BLOQ 8.5 BLOQ 53.1 BLOQ 54.1 BLOQ 56.9 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ ' BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ . BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ " BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ ' PFOS (499) Corrected for Smpl Prep (nglmL) 185.5 130,0 139.7 635.5 614.0 571.7 732.1 807.7 824,4 688.4 757.0 653.3 465.5 415.0 388.7 693:2 599,1 660.2 25.6 96.7 117.6 64.7 530.8 540.9 569.4 .... ADveev,,Satnndd %CV 152 29.61 19.5% 607 32.49 5.4% 788 49.18 6.2% 700 52.70 7.5% 423 39.03 9.2% ' 651 47.78 7.3% 100 16.68 16.7% 547 20.02 3,7% Corrected for sample prep. Amount(nglmL)" 10 CoNidenltal Average (ppb) : Stnd. D.: SL-I. LM PFO_. 64.3 NA PFOS 553.4 220 12/17/2002 SL-2, LM PFOS Average (ppb) : Stnd. D.: 280.8 251 Pmge 14 o121 Environmental Laboratory Page 54 of 276 Report E02-0443 , _ Tenn. River Valley Samples Combined E02-0443 CatFish Data Table PFBS (299) PFHS (399) LIMS # _Sample Name 42777 42778 42779 42780 42781 42782 42783 42784 42785 42786 42789 42790 42791 42792 42793 42794 42795 42796 42797 SL-1; C-1-1 SL-1; C-1-2 SL-1. C-1-3 SL-1. C-2-1 SL-1. C-2-2 SL-1. C-2-3 SL-I. C-3-1 SL-1. C-3-2 SL-I. C-3-3 SL-1. C-4-1 SL-1. C-4-2 SL-I. C-4-3 SL-1. C-5-1 SL-1. C-5-2 SL-1. C-5-3 SL-1. C-6.4 SL-I. C-6--2 SL-I. C-6-3 SL-2; C-1-1 SL-2; C-1-2 SL-2. C-1-3 SL-2. C-2-1 SL-2. C-2-2 SL-2. C-2-3 SL-2. C-3-1 SL-2. C-3-2 SL-2. C-3-3 SL.2. C-4-1 SL-2. C-4-2 SL-2. C-4-3 SL-2. C-5-1 SL-2. C-5-2 SL-2. C-5-3 SL-2. C-6-1 SL-2. C-6-2 SL-2. C-6-3 SL-2. C-7-1 SL-2. C-7-2 SL-2. C-7-3 SL-3; C-1-1 SL-3; C-1-2 SL-3. C.1-3 SL-3, C-2-1 SL-3, C-2-2 SL-3. C-2-3 SL-3. C-3-1 SL-3. C-3-2 SL-3. C-3-3 sL-3. C,,_JI SL-3. C-4-2 SL-3. C-4-3 SLo3, C-6-1 SL-3. C-5-2 SL-3. C-5-3 SL-3. C-6-1 SL-3. C-6-2 SL-3. P--,-63 Amount ng/ml_ BLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOC} BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ BLOQ., BLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ BLOQ SLOG BLOC] BLOQ SLOG BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SLOG Amount ng/mL BLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ BLOC] BLOQ BLOQ BLOQ BLOQ BLOQ SLOG BLOC} SLOG BLOQ BLOC} BLOQ BLOQ BLOQ BLOQ BLOQ BLOC] SLOG BLOQ BLOC) BLOQ BLOQ BLOQ BLOC} BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SLOG BLOQ SLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SLOQ BLOQ BLOQ PFOA (4132 Amount ng/mL ALGa BLOC] BLOQ BLOQ SLOG BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ SLOG 8LOG BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ SLOG BLOQ RLOQ BLOQ SLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ BLOQ aLOQ BLOQ SLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ SLOG SLOG BLOQ BLOQ BLOQ BLOQ BLOQ Amount nglmL 5.9 5,3 5.2 4.4 4.2 3.9 7.0 7.1 7.4 3.9 3,7 3.8 9.1 9.1 8.8 7.0 6.9 7.0 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SLOQ BLOQ _, BLOQ BLOQ BLOQ BLOQ SLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ BLOQ BLOQ SLOQ BLOQ '-BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ FOSA (498) Corrected for Smpl Prep (n_l/mL) 58.7 53.5 52.0 44.5 41.7 39.1 70.5 70.6 73.8 39.3 36.7 38.2 91.0 90.7 875 69.8 69,1 69,8 Ave, Stnd Amount DeV,%Cvand nglmL 54.7 349 6.4% 41.8 2.67 6.4% 71,7 1.85 2,6% 38.1 1.30 3.4% 89,8 1.95 2.2% 69.5 0.41 0.6% 11.2 10,5 10.0 9.8 9.2 8.6 16.1 17.9 19.2 17.1 16.2 16.6 8,I 8.0 7.8 5.9 6.0 5.9 BLOQ BLOQ BLOQ BLOQ BLOC} BLOQ BLOQ SLOQ BLOQ BLOQ BLOQ SLOG BLOQ BLOQ BLOQ 8LOQ BLOQ BLOQ BLOQ BLOQ BLOQ 1.9 1.9 1.4 1,2 1.1 1.2 BLOQ BLOQ BLOQ 3.7 3.5 4.0 BLOQ BLOQ BLOQ BLOQ 2.3 2.3 PFOS (499) Corrected for Smpl Prep (n_mL) 112.1 104,7 100.3 97.6 91.8 86.1 161,2 179.4 192.4 171.5 161.9 165.8 80,8 80.2 77.5 58.8 59.7 58.7 18.8 18.7 14.0 11.5 11.5 12.2 35.9 35.1 40.4 23.5 23.2 Ave, Stnd OeV,%cvand 106 6,00 5.7% 91.8 5.77 8.3% 178 15.67 8.8% 166 4.82 2.9% 79.5 1.74 22% 59.1 0.57 1.0% 17.21 2.75 16.0% 11.73 0,44 3,7% 37.45 2.72 7.3% 23.32 0.19 0.8% Corrected for semR_ prep. Amount (ng/mL)" 10 Average (ppb) : 5tnd. D.: SL-1, C FOSA 60.9 18.6 PFOS 113.4 45.6 SL-3, C PFOS Average (ppb) : Stnd. D.: 22.3 10.6 Ef_com_ntaLial_'ltOvy t2111/2002 Page15ol21 3M Environmental Laboratory Page 55 of 276 Report E02-0443 - - Tenn. River Valley Samples Report E02-0443 - - Tenn. River Valley Samples | Report E02-0443 - - Tenn. River Valley Samples Report E02-0443 "- Tenn. RiverValley Samples ReportE02-0443 . _ Tenn. River Valley Samples E02-0443 Condensed River Water Data Table PFBS (299) InJ. Vol. Amount OnColumn Adjusted for Adjustld for Sample Prop, Average LIMe # Sample Nmme 38025 SW01 __?a.o?.s_.__s2,lwop...zD, 38033 SW03 38034 SW03-Du__ 38037 SW02 tuL) 20 20 20 . 20 20 (n_/mL) 3.0 3.7 <LOQ <LOQ <LOQ InJ. VoL (ng/mL) 1.5Q 1.85 Ip?lmL ) 75 93 (pglmL) 64 <LOQ <LOQ _kd|ustl_dfor fo|. Vol (ncl/mL_ For 20 uL injections = Amount / 2 38038 StN02-Dup 20 36028 SW01-Med 2 38030 FSC01-Med 2 38036 SW03-Med 2 38040 b-'V_/02-Med 2 38042 FSC02-Med 2 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ For 2 uL injecbons Amount" 5 PFHS (399) 38025 S_N01 20 38020 S_N01-Du_ 20 38033 SW03 20 38034 S_/03-Dup 20 7,7 6.0 <LOQ 0.3 3.86 5.96 0,13 193 196 199 6,6 6.5 Adlu$ted for Saml)le Pine |m_/mL_ = (Adjusted for In_.Vet. / 20)" 1000 38037 SW02 20 38038 S1N02-Dup 20 38028 SW01-Med 2 0.4 0.2 382.6 0.20 0.12 1963 9.8 8.0 6.2 20 is the factor of Original concentration 1000 is the convemion frorn ng to pg, 38030 FSC01-Med 2 424.9 2124 t 38036 SVV03-Med 2 404.9 2024 38040 SW02-Med 2 415,9 2079 ! 38042 FSC02-Med 2 413.1 2066 " 38025 / SW01 PFOA (413) 20 21.3 10.66 533 550 3802.6 i ._. S.W01_-__..up.__ 20 38033 " SW03 20 22.7 <LOQ 11.33 566 <LOQ 38034 SWO3-Dup 20 <t.OQ 38037 SW02 20 <LOQ <LOQ 38038 SW02-Dup 20 <LOQ 38028 SVV01-Med 2 388.4 1942 38030 FSC01-1ded 2 427.9 2139 38036 SW03-Med 2 398.5 1992 38040 SW02-Med 2 407.8 2038 38042 FSC02-Med 2 416.9 2085 F0 ..... ,,. . il 38025 SW01 20 S1.0A (4981 0.48 24 25 38026 SVVO1-Du_ 20 1.0 0.51 26 38033 SW03 20 <LOQ <LOQ _ 38..9.34__... _3-puu_ 38037 SW02 20 <LOQ 20 <LOQ 38038 SIN02-Dup 20 <LOQ 38028 SW01-Med 2 302.1 38030 FSC01-Med 2 300.2 38036 SW03-Med 2 38040 SW02-Med 2 38042 FSC02-Med 2 324.5 299.2 308.3 1511 1501 1623 1496 1542 <LOQ 38025 __3e9_'_. 38033 SW01 s_..o_ SVV03 PFOS (499) 20 18.5 20 2o.8 20 <LOQ 9.25 lO.4O 462 52o 491 <LOQ 38034 SW03--Oup 20 38037 S_/02 20 38038 SW02-Dup 20 38028 SVV01-Med 2 38030 FSC01-Med 2 38036 SW03-Med 2 38040 SW02-Med 2 38042 FSC02-Msd 2 <LOQ <t.OQ <LOQ 361.8 423.7 365.3 358.0 426.8 1809 2118 1826 1790 2134 <LOQ 3M C_d_al 3M Environmental Laboratory 12/17/2002 _ 20oq21 Pa_e 6r) nf ?76 ReportE02-0443 . _ Tenn. RiverValley Samples E02-0443 Tenn. River Valley Samples Summary Table Location Averages Catfish, Sample <LOQ < LOQ <LOQ 60.9 113 Location 1 Catfish, Sample Location 2 <LOQ <LOQ <LOQ <LOQ <LOQ Catfish, Sample <LOQ <LOQ <LOQ <LOQ 22.3 _,! Location 3 , Large Mouth, Sample <LOQ <LOQ 64.3 <LOQ 553 Location 1 i Large Mouth, Sample <LOQ <LOQ <LOQ <LOQ 281 _t Location 2 Large Mouth, Sample Location 3 <LOQ |l <LOQ <LOQ <LOQ <LOQ i Small Mouth, Sample Location t <LOQ <LOQ <LOQ <LOQ <LOQ PFBS PFHS (pglmL) PFOA. _ FOSA _._g/mL_ PFOS __pq/mlJ River Water, Sample 84 Location 1 196 550 25 491 ! RiverLWocaatteiro,nSa2mple <LOQ 8 <LOQ <LOQ <LOQ ii River Water, Sample Location 3 <LOQ 7 <LOQ <LOQ <LOQ PFBS PFHS (nglmL):_ _'- (ng/mL_ EgEi River Sediments, 576.9 130.5 732.4 t439.0 3132.3 Sample Location 1 . River Sediments, Sample Location 2 436.9 <LOQ <LOQ 141.4 457.3 River Sediments, 452.0 <LOQ 130.5 68.0 - 416.2 : Sample Location 3 = .'_ The FishT_ssureesultsarecalculatebdytakingtheaverageoftheaverages. I Pleasereferto CombineLdargeMouthandCatfishDataTablesforaverageos f samples. 3MConfidential 3M EnvironmentalLaboratory 12/1712002 Page21of 21 Page 61 of 276 Report E02-0443 Tenn. RiverValley Samples u_ "6 & Report E02-0443 Tenn. River Valley Samples "6 ReportE02-0443 Tenn. River Valley Samples 3M EnvironmentalLaboratory Pa_e 64 of 276 Report E02-0443 Tenn. River Valley Samples Lt_ "5 _r & 3M Environmental Laboratory Page 65 of 276 Report E02-0443 - - Tenn.River Valley Samples "5 ReportE02-0443 . _ Tenn. RiverValley Samples ATTACHMENT C: SAMPLE CHROMATOGRAMS 3M Environmental Laboratory Page 67 of 276 ReportE02-0443 . _ Tenn. RiverValley Samples Data File: DUDE0056.D Report Date: 27-Aug-2002 13:27 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\DUDE0056.D Lab Smp Id: SL-I. LM-I-3 Inj Date : 26-JUN-2002 23:16 Operator : mla Inst ID: dudejr.i Smp Info Misc Info : Tenn. : River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\D020626extra Meth Date : 27-Aug-2002 13:22 dudejr.i Quant Type: ESTD Cal Date : 26-JUN-2002 22:00 Cal File: DUDE0049.D Als bottle: 43 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compo_md8 IIIl=lUllllllllllllltlll=" 18 PPBS (299) ! 20 _PH.q (399} i . 21 PFOA (413) ". I !_ 32 FOSA (498) ; 23 pP13_ (4_9) QUANT SIG MASS lilt 299 299 299 399 399 413 399 413 4_8 498 499 499 RT lilt 3.388 3.176 3.723 3.805 3.401 EXP RT I=t==lll 3.3al 3.381 3.381 3.792 3.792 DLT RT =====l== 0.007 -0.205 0.342 0.013 -0.3S1 RBSFONSR llllllll 11884 2064 1527 9981 4708 CONC_NTRAT ON- COLUMN (ng/mL) IlllllN $53.334 553.695 553.714 809.355 809.488 IONS FINAL (ng/mL) Illllll 5S3 5S4 554 609 809 4.003 3.976 3.873 4.755 4.441 4.174 4.605 2.890 3.792 3.990 4.762 4.7G2 4.174 4.174 0.013 0.184 -0.117 -0.007 -0.321 0.000 0.431 15342 4267 5385 05375 984 1903432 19078 837.253 809.499 837.750 0.11S_8 1917.31 13.9702 1680.28 837 809 638 0.116 1920 14.0 1680 Ex__C=to..-.'/rO:: riginal Initial Data 3M Environmental Laboratory Page 68 of 276 Report E02-0443 - - Tenn. River Valley Samples I_ataFile; \\EtstaPget%taPget%che_\dudeij\PI.}O20626Extra_ted.b\DUOEOO56.D 5.2_ 5.0_ 4.8" 46" 4.4_ 4.2" 40i 3.83.6_ 3.4: 3,2! \bEtstarget_target\chem_dudeij_r).206ZGExtraotedb,_UDEO056.D ,_ 2.e- 2.4" 2.220" 1.8-_ Page 2 1.2" i.O" I o.8- :'_ 0.6- o0..24- : I_1 +" o'._ i;$" i8 PFBS (299) I =! _ Illl ,_ II |J LL] _'.6 2'.o _'._"3"_'_'6 ";._';._"_'._; _'._+_'._, 6'.6 Hin _,:o y.s_ e'o e'.6"_,'.o " 4ol5" Ion 299.00 3.9" 3.6" 3.3: :':I _ 32..07-- 2.4- ; > 2.t" r_ i.e" _._-_ i + - - i i 1 , i 3.00 3.20 3.40 3.60 3.BO Hie 2opRO<S:_ 1on 399o00 + "+ 2.6" 2.4-". 2.2 ,,, 1:t..6e _. 1.4 t2 t.0 0.8 .6 I ,,,; i i i . + i 3.40 3.60 3.80 4.00 4.20 M|n ExacCt c77_: Ori;inal 3M Environmental Laboratory _ .......... Report E02-0443 TI I Tenn. River Valley Samples Data Rile." %%Etstar_et\target%chem\dude_roi_I)O20626Extraoted.b_DU_EOO56.D 21 PFOA (413) Ion 413.00 3.6" o 30 i I 22..17-- o 1.5-." 3.60 j ....... 3.8_in4.00 4.20 4.40 FOSA (498) Io_ 498.00 5o5_ 4o5_ 4.0" ^ 3.5-'.' > 2.0- ,; 10..55_= , ,',!_ 4.40 ,__, 4.60 4.80 H;n 23 PFOS (499) '/, 5.00 5.20 Ion 499..00 4.03.6_ 28-." 2.4- __zt6."o" 4i..z4_" _I _ 0.4-." : , o. 3.80 I I - | 4.00 4.20 Hin v I I_l - o - n, 4.40 4.GO I i Pa_e 3 ExacCt opy(_fO,_--,, _ Initial "_' '_''/" Date 3M EnvironmentalLaboratory Page 70 of 276 ReportE02-0443 Tenn.RiverValley Samples Data File: DUDE0058.D Report Date: 27-Aug-2002 13:27 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\DUDE0058.D Lab Smp Id: SL-I. LM-2-2 Inj Date : 26-JUN-2002 23:38 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MI.d_.. 20 Jun 02 Misc Info : Comment : Method : Meth Date : Cal Date : AIs bottle: Dil Factor: \\Etstarget\targetkchem\dudejr.ikD020626Extracted.bkD020626extra 27-Aug-2002 13:22 dudejr.1 Quant Type: ESTD 26-JUN-2002 22:00 Cal File: DUDE0049.D 45 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Coat.de mnmm.mmmmmmmnmmmmimmmmm.lm 18 PPBS (299) 20 P_B (399) 21 pFOA (413) i_ 22 FOSA (498) i_ 23 PFOS (499) ii i QUA,'q'I"SIG RU_-%9 mmm= 299 299 299 299 399 3_9 413 413 498 499 4S9 RT mm.m 3.388 3.190 3.306 3.723 3.805 3.545 3.167 4.229 _P RT DLT _T mummmli..=l.mmim 3.381 3.311 3.381 0.007 -0.191 *0.075 3.381 0.342 3.792 3.792 0.013 -0.247 3.990 3.990 -0.123 0.239 4.762 4.174 4.605 4.762 4.174 4.174 0.000 0.000 0.431 RBS_NSE ms.nm._= 11577 4900 5158 2027 13422 2338 47254 2493 _42653 3385486 164G6 C_:_CE_TI ON- _L_N (ng/mL) mmmm..m 553.345 553.58K 553.581 553.596 809.259 809.548 0.655_? 837.894 2.965?5 61.4006 1680.36 ONS FINAL (ng/mL) n.mmmmm 553 5_4 554 554 809 K10 0.655 838 1.96 61.4 1610 I ExacCt c;:fofOriginal . _.m,' _z..-. _i! Initial Date 3M EnvironmentalLaboratory Page 71 of276 Report E02-0443 Tenn. River Valley Samples Data FiXe" XXEtstargetX_aPcet%chemXdudejr'.i_DO20626Ext_'acted.bXDUDEO058.]) 3.43.23,- 2.8- 2.6-' \\Etstar'etXtael:e t_cheMXdudej r, l\DO20626Extr 2,4" a2-_ 2,0_ _, _.8- _ 1.62 >- 1.42 1.2- act ed, bXDUDEOSB, ]D Page 2 il o0..64;;. 00,.82-- "11111 II .... i .... 0,5 i .... 1.0 | .... 1o5 _ .... 2,0 . .... 25 i r.J = .... 3,0 __l 1 II = .... a .... 35 4,0 I_111, i .... 4,5 Hin = .... 5,0 IIII i .... i .... 5.5 60 i .... B .... 6,5 70 i .... 7,5 i .... 8.0 i .... 85 i .... ?0 18 PF_S (299) 4.5" i Ion a99,00e_ ij 336._, '1 o Po t_ , 3.0- _ ,_ _ 22.7.: 4 ,P_ /_I 1.9- : 4t..25-." _r_ >- 21..12:!_ i - i i !..- i. 3.00 3,20 3.40 3.60 3,80 20 PFHS (399) Ion 399.00 2.,- _ _," .'. 2.2_ [I 20: ,_ _.8" "4i " I k/\ "1,2J I J I) | F.x,_CcCt 'Zr:':Origins} Initial Date i.o-:_ 3,40 3,60 3,80 4.00 4,20 H_n 3M Environmental Laboratory Page 72 of 276 Report E02-0443 Data File: %_EtstaPget%target%che_udeje.i%DO20626Extracted.b\DUDEOOSS.D 21 PFOA (413) Ion 413.00 4.5- ":4.2: 3.S" _ 3.3- o _.0- 32.._7-:: . 2,,4"_ At /V / L i 1.5 - - i | i , + - , I 3.0 3.90 4.00 420 4.40 Htn 22 FOSA (4_8> Zon 4_.00 ; !t;; ! i I :'I + 1,0" " i 0.6822 ,_,o )" 0.4" _r I 0,2-i" 4.40 , 4,60 4+8 HSn 23 PFOS (4_9> ,j 5.00 5,20 " M I I I^ ,5..0o- _: _v4.3o.:0i 2.0-:" ,=4..%= : o, 3.80 t . n o- i 4.00 4.20 4,40 Hin t I o 4._ J t .:i _ Tenn. River Valley Samples PaKe 3 ExacCt epyofOrig!n_] .L_;"c+ _:_l"__e._L-_ IniUal Date 3M Environmental Laboratory Page 73 of 276 Report E02-_43 . _ Tenn.River Valley Samples Data File: DUDE0063.D Report Date: 27-Aug-2002 13:27 "- Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\DUDE0063.D Lab Smp Id: SL-I. LM-3-2 Inj Date : 27-JUN-2002 00:33 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Misc Info : Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstargetktarget\chem\dudejr.i\D020626Extracted.bkD020626extra Meth Date Cal Date : 27-Aug-2002 : 26-JUN-2002 13:22 dudejr.i 22:00 Quant Type: ESTD Cal File: DUDE0049.D Als bottle: 49 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub !I ; ! _ ._ ; 'i .._ Concentration _nd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compounds ll=llllli = IIIIIInllilimill 10 PFBS (299) 20 PFHS (396) 21 PPOA (413) 22 POSA (498) 23 PPOS (499) QUANT SIG MASS I=nn 299 299 299 299 399 399 399 413 413 499 49J 499 499 RT nnll 3.388 3.176 3.723 3.812 3.798 3.545 3.976 3.997 3.853 4.762 4.414 4.174 4.605 _P RT nnlnxl== 3.381 3.381 3.381 3.381 3.792 3.792 3.793 3.990 3.990 4.762 4.762 4.174 4.174 DLT RT nullnnnn 0.007 -0.205 0.342 0.431 0.006 -0.247 0.114 0.007 -0.137 0.000 -0.340 0.000 0.431 RES_NSE m=n=lnnw 11469 2575 1432 378 9750 3036 4357 16533 $476 236312 STO 3964776 26340 _NCEN'I'I_TIONS ON- _L_N FZNAL (_9/mL} Ilillll 553.349 (ng/mL) lllll== SS3 563.676 563.716 553o7S6 809.361 554 554 554 BO9 809.$30 010 809.497 009 837.243 037 837.745 836 4,9011S 1917.31 80.7677 1600.07 4.98 1920 80.8 1680 ...i ExacCt e,_oyfOr!_inal _ Dat8 3M EnvironmentalLaborato_ Page 74 of276 Report E02-0443 . _ Tenn. River Valley Samples l_ata File: %_Etstar_etXta_etX_m_dejr.iXDO20626Extract_,b%DUDEOO63.D Pal;e 2 \_Etstafcet\targe_chem\ciu_ej r, i\OO20626Extract ed, b_gUDEOO6D3. 2,6- 2o5_ 2,4-." 2,32.2_ 2.14 2.0-." t.9" 1.8" t.7: 1.6" 1o5_ t.4" 1.31o2_ 1.0_ 0o9_ 0.8. 0.7" 0.6_ 0.54 0.4_ 0.3" o,2-: O.'t" t =i I I _1 . I . 1,,J u llJ I t. I I "" "$;_""_'._";' i'._ ""z:o ' 2"5""3'.o"' _'._"":Ko'";K_' "_'.o""s:_'"_;;'" Cs'" _'.o "_'_'" ;;.o" 8'.B",'.o' ' Hin 18 PF]_ <2_9) Ion 299.00o_ 3.6" t 3.0" ' _ z.?" 'i! _ 2.4: _. _ _; i l._: , 1.2 : 1"5i. _ 3.0 3.20 3,40 3.60 3.80 Hiq 20 PFHS (3J_) Ion 399.00 ' 2.4-." I 2.2; ' =.s_. II _ I[ I[ 9 Exact Cop_, {;f Ori_i_ld,I T I i/ \ '4 3,40 3_0 3,80 4,00 4.20 Hin 3M Environmental Laboratory P_,_ "_5_f ?Tn Jl II ReportE02-0443 Data File: %_EtstaPgetNta_[et%chemNdudejr.i%9020626Extracted,b%DUgE0063.D 2t PFOA (413) 3.9- 3._,- 3 3 -." 3.0-' Ion 41300 . "; 22.7.",-: =_ 'v_ 2.i: P*o i.zJ 0,9- ........ , .. . , .. . , . 3.60 3.80 4.00 4.20 4.40 22 FOSR (498) Ion 499.00 7.0- 6.o_ 4 i 4.0>" 2.0J l-oi 4 5.0" " l ;i l L o ' i = ..I.. J 4.40 4.60 4.80 5.00 5.20 H|n 23 PFOS (499) , s.oi : Ion 499._00m '. 9.0" ' 7.0" ! ,oO 'I .!.I i _4.0.o_ i 2.o! l.O_: 3.'_ t/ ,i._ ,i._ i I_,L,rj ,i.'4o,i._ Tenn.River Valtey Samples I II ] Pal_e 3 3M EnvironmentalLaboratory Page 76 of 276 Report E02-0443 .. Tenn.River Valley Samples Data File: DUDE0068.D Report Date: 27-Aug-2002 13:27 Page 1 3M Environmental Laboratory Data file E02-0443, Tenn. River Valley Samples : \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\DUDE0068.D Lab Smp Id: SL-I. LM-4-2 Inj Date : 27-JUN-2002 01:28 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Misc Info : Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment Method : \\Etstarget\targetkchem\dudejr.i\D020626Extracted.b\D020626extra Meth Date : 27-Aug-2002 13:22 dudejr.i Quant Type: ESTD Cal Date : 26-JUN-2002 22:00 Cal File: DUDE0049.D Als bottle: 52 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Cpnd Variable Formula: Amt * DF * CpndVariable Local Compound Variable _om[:_ounds =.....===Rmmmm=wmmmm..mm=m 28 PPBS (299) 20 p1:3-IS (399} 21 P-mOA 4413) 22 FOSA (498) 23 PPOS (499) QUANT SZG MJ_S m.=m 299 299 299 399 39S 398 423 498 499 499 499 RT =.== 3.388 3.183 3.723 3.798 3.3S4 3.S59 3.997 4.762 4.174 3.8_7 4.60S EXp RT ...=.=.= 3.381 3.381 3.381 3.792 3.792 3.792 3.990 4.742 4.174 4.174 4.174 DLT RT n_w.:m.. 0.007 -0.198 0.342 0.006 -0.438 -0.2_3 0.007 0.000 0.000 -0.307 0.431 RESPONSE :==._=.. S1072 2350 1509 49154 415 3064 162661 9787S. 3814537 152g 16518 CONCENTRATIONS ON-COLUMN F IbTAZ, (n /mL) ..=n_:= 0.83332 $53.684 SS3.715 0.63726 809.596 808.529 6.42649 0.51796 7S.6964 1600.79 1680.35 (ng/mL) ==m_.=. 0.833 554 5S4 0,637 810 810 6.4] 0.518 75.7 1680 1680 ExacCtop:/oOfri_inaJ Ir_al Date 3M EnvironmentalLaboratory Page 77 of 276 Report E02-0443 II Tenn River Valley Samples Data File: %%Etstar:et%target%cheR\dudejr,i\Dozo626Extraoted.b%I_EOO68.D 1.6i %_Etstar:et_taret\cheM_durd.eij\DO20626Extracted.b_J3UI)EDO068. Pace 2 1.4i.31.2- t..0 2" <=0.9-" ox 0.8: >, 0.7- 0.6; 0.5- o4 i 0.3-_ :0 .:1,-' .... I --Li ,.... i .... | .... , .... i ........I.... ,_ 0.5 i.O i. 2.0 2. 3.0 i 18 PFBS (299) 1.6: i.4: Ion 29900 r_ ;UL _, t-'l i .... 3.5 4.0 p .... 4.5 Htn , .... 5.0 I i I._... I ,-i .... 5.5 6.0 J .... 6.5 = .... 7.0 i .... 7.5 i .... 8.0 i .... 8.5 _.-.'; 9.0 1.2- i i.o" :J= 0.8" :id ! OG2 . i i - i - i... 3.00 3.20 3.40 3.60 M|n i. 3.80 20 PFHS(399) Ion 399.00 I i.i; " i 0.94 o0.'5.6i_i 0.4,'= 0.3,; o.z,: 3.'4o_.'6__.8_4.'_ _.z_ __",m_./L_.___- ./__'_- tr_tiaJ Or_t_ 3M Environmental Laboratory Page 78 of 276 Report E02-0443 Data File: %%Etstaret\tarcet\che_%dudejr.i_JOO20626Extracted.b\DUDEOOGB.D 2t PFOR (413) 4.o_ z_ 4].00 N 3.22.6:. 22..04-"- > _ .2 -.' 0.8" 0.4_.,,,.i . ........ 3.60 3.80 4,00 HLn 22 FOSA (498) Ion 498.00 7.0_ 6.0" 5.0-." ! 4.o ,,...-_,. 4.20 440 :_ _ 3.o-2:-._o._.,i.o.. !., _ Il 4.40 4.60 4.80 5.00 .20 H_n 23 PFOS (499) e.o_ Ion 499..00 _. 7.oi :{ 6.0" 5.0-': "_ 4.0" _.o_".1. , _.t. ,, J ,'-- 3.80 4.00 4.20 4,40 Htn i _'_ 4,60 i "l; Tenn. River Valley Samples PaCe 3 E_acCt opyofOrJ=_ina! laJl_ai Bate 3M Environmental Laboratory Page 79 of 276 Report E02-0443 . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02062S.b\DUDE0058.D Report Date: 09-Dec-2002 13:07 Page 1 3M Environmental Laboratory Data file : Lab Smp Id: Inj Date : Operator : Smp Info : Misc Info : Comment : E02-0443 Tenn. River Valley Samples \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0058.D SL-2. LM-2-1 29-JUN-2002 02:15 mla Inst ID: dudejr.i Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Method : \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m Meth Date : 09-Dec-2002 Cal Date : 29-JUN-2002 13:01 dudejr.i 00:48 Quant Type: ESTD Cal File: DUDE0050.D Als bottle: 28 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compounds QUANT SIG MASS ET EXP RT DLT RT RESPONSE CONCENTRATIONS ON- COL_ FINAL (ng/mL) (ng/mL} i$ pFBS (299) 20 PFHS (399} 21 PFOA (413) 22 FOSA {498) 23 PFOS (499) L:_ 299 3.388 3.388 0.000 15144 569.524 570 299 3.383 3.388 -0.205 2946 569.996 570 299 3.757 3.388 0.369 2208 570.025 570 399 3.805 3.798 0.007 10047 786.229 786 399 3.545 3.798 -0.253 540 786.477 786 413 4.004 3.997 0.007 25432 815.277 815(M) 498 4.776 4.769 0.007 65904 1885.85 1880 499 4.181 4.174 0.007 1348329 2.56372 2.56 499 4.605 4.174 0.431 20726 1659.69 1660 i QC Flag Legend M - Compound response manually integrated. ii ExacCt opayfOriginal _tiaJ Date 3M Environmental Laboratory Page 80 of 276 Report E02-0443 Tenn River Valley Samples Data File: %_Etstarget%taPet%che_\duckejr.t\)O20628.b\DUDEOO58.D Pace 2 _\EtstaPzet_taret\ch_dudej r i \D020629. b\DUIEO058D. 3.3 i 3.24 30_ 2.94 2.S_ 2.7_ 2.6-' 2.5-_ 2.4_ 2.3_= 2.2_ 2.i3, 2.0" i.9=' i.7" li..68"4 >" _..4_ 1.3_' 121 t,0._ 0.9._ : 0,7.:' 0,64 :i o.s_ _, o.4._ o.3._ o.2J _1I JJ"_JI I .... _ __ I ,T .................... I =.. * .... I .... = .... , .... = .... 0.5 i.O 1.5 2.0 2o5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 H|n 18 PF_S (299> 3,6- Ion 299.% ro ! 3.3:. r_ i 3.0-" 1 z,4: '; t .,.e- _r _'_i ! 2o.t9"-.: i0.2,6-'"_ i 3.00 i i 3.20 3.40 Htn . i | 3.60 3.80 20 PFHS(399) ; Ion 399.00 ' ::.:: :.z- _ _.._ I/_ 0.6:_ - B. 3.40 " - - i m 3.60 3.00 Pl|n - i . | - 4.00 4.20 _al Date aact coo,o:,fori,_ina! 3M Environmental Laboratory Page 81 of 276 Report E02-0443 Data File: \%Etstarget%target%cheM\dudeJr.lM))20628.b%DUDEOO58.D 21 PFOR (413) 3,93.s" 3.3- 3.,: 2.7- ][on 413.00 .t " 1i , : >" 1.8" t.5" 1.2 i . i i |-., 3.60 3.80 4.00 4,20 Htn 22 FOSR (498) 604 5.5_ 5.o_ 45 i 4.0_ Ion 499.00 w, 4,40 3.5! 2.4 " >" t.5" 3"i 1* i 0.64 ;_ 4.40 I 4.60 4.8,> H(n 23 PFOS (499) i .00 5.20 3.3-: 3." 2.7" 2.42.1: <_ 1,8" v 1.2: > 0.9: o.6_ 0.3" 3.80 Ion 499.00 i 4.00 4.20 Htn 1 TL_ 4.40 4.60 i ,. I . _ Tenn. River Valley Samples ..o Page 3 ExacCto' oo:,f,_": ,.3,.t.:_.; Initial Oate 3M Environmental Laboratory Paae 82 of 276 ReportE02-0443 Tenn.RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0064.D Report Date: 09-Dec-2002 13:07 Page 1 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0064.D Lab Smp Id: SL-2. LM-3-2 Inj Date : 29-JUN-2002 03:21 Operator Smp Info Misc Info : mla : Tenn. : River Valley Inst ID: dudejr.i Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m Meth Date : 09-Dec-2002 Cal Date : 29-JUN-2002 AIs bottle: 33 Dil Factor: 1.00000 13:01 dudejr.i 00:48 Quant Type: ESTD Cal File: DUDE0050.D Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable ,;,| Compoun_ 18 P_S (299} .i " i i :_ 20 P_ 21 PFOA (399} (413} 22 F_A 23 P_S (498) (499} ] ! QC Fla 9 Legend t ! M - Compound response QUANT SIG MASS 299 299 299 399 413 498 499 499 RT EXP RT DLT _ RESP_SE _NCENT_TIONS ON- _LUMN FIN_ (_/mL) (ng/_) 3.401 3.2_0 3.771 3.818 4.017 4.785 4.194 4.625 3.388 3.388 3.358 3.798 3.%97 4.769 4.174 4.174 0.013 -0.178 0.383 0.020 0.020 0.020 0.020 0.451 22037 3476 3793 17063 38939 98985 1627015 1774 569.257 569.976 569.964 0.08850 814.559 0.72476 11.7650 1G60.28 569 570 570 0.0885(M) 814(M) 0.725 11.8 1660 manually integrated. i EYaCtCo2,,r;n_,.b_n_,_ 3M EnvironmentaLl aboratory Page 83 of 276 Report E02-0443 Tenn. River Valley Samples I)a_o File, %%Etstarl;et%tartet\che_\dudejr.t\D20628.b\_UDEO064.1) 4o2-: 4,0- 3.e- 3.6_ 3.4" 3.2_ 3.02.8_ 2.6-" 2.4" i a._i 20_ >. t.8: _..6- .., 1.4; i.2._ t.0i _Et,$t_-i_et,\tar get _he_\dudej r. 1%1_020629. b\I_UTEO064. D :_ o.6- 0.4" 0.2" o.eis"1 ;_J_ i _L._-_ J4J_ , o.s 1.0 _'" z:_" _,'_"3'._'"_:_ ................... 6.0 HJn t8 PFBS (299> 4,4-." 4.03.6_ Ion 299_'_ '_4 32..28- " '_ __ 2.0- 0,8" = . i - i .... n. 3.00 3.20H_n3.40 3.60 -o0 3.80 20 PFHS (399) 3.2_ lon 399.00 3.0-. a.e_ .; 2._- i 2.4" z.z:. (_ 2.0" _..2-: 3.40 3.60 3.80 4.00 4.20 Pa_e 2 _.,.C,_ot pyo_.OrlglnaJ 3M Environmental Laboratory Page 84 of 276 Report E02-0443 Data File: %_EtstaPcet%target%chem_dudejr.l%I>)2062B.b\DUDEOO64.D 21 PFOR (413) 5.2" 4.8" 4.4, 4,0-_ Ion 4't3.00 p. 3.6- o 3.2" 2.8-" >" 2.4_ 2o0_ t.6" t.2-:. , . . . _ . . . , . . . _. . . , . 3.60 3.80 4.00 4.20 4.40 Hin 22 FOSR (498) I0_ 499.00 40, 3.6_ i! 3.2, I z.s-: _ 2.4" . ! _ 2.0" .r i _ 1.2, " 0.8-: 0.4" - _ o i i .... 4.40 4.60 4.80 5.00 .20 Htn 23 PFOS (499) Ion 499,00 I 4.0: ', 3.6, 3.2" i; 2.8, : 2,4" 2.0, /L " _1: :,-, J0..o82:.: oJ 0.4: _; : . . , . . . I ..... _. , . . p.l 3.80 4,00 4.20 4.40 4,GO ,,, H_r_ . _ Tenn. River Valley Samples Pa." 3 EXBCt Cop;,_-lf Or;.:.j"in_--:. _niUaJ Date 3M Environmental Laboratory Page 85 of 276 Report E02-0443 Tenn. RiverValley Samples Data File: \___=_Li,\\Etstarget\target\chem\dudejr.i\D020DzS.b\DUDE0070. Report Date: 09-Dec-2002 13:07 D Page 1 3M Environmental Laboratory Data Lab Inj file : Smp Id: Date : E02-0443 Tenn. River Valley Samples \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0070.D SL-2. LM-4-3 29-JUN-2002 04:26 Operator Smp Info Misc Info Comment : mla : Tenn. : : River Valley Fish. Inst ID: dudejr.i Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Method : \\Etstarget\target\chem\dudejr. Meth Date Cal Date : 09-Dec-2002 : 29-JI/N-2002 13:01 dudejr.i 00:48 Als bottle: 37 Dil Factor: 1.00000 i\D020628 .b\D020628 .m Quant Type: ESTD Cal File: DUDE0050.D Integrator: Falcon Compound Sublist : all. sub .,_ Target Version : 4.12 , i Concentration Formula: Amt * DF * CpndVariable i Cpnd Variable t Local Compound Variable CompOunds 10 PFBS (299) : 20 PFHS (399} 21 PFOA (413) .} 22 FOSA (498) l 23 PFOS (499) . :_ QUANT SIG MASS 299 299 299 399 413 498 499 499 499 RT EXF RT DLT RT RESPONSE CONCENTRATIONS (_ - COLD_ FINAL (ng/mL} (ng/mL) 3.388 3.183 3.757 3.805 4.003 4.776 4.174 3.805 4.605 3.388 3.388 3.388 3.798 3.997 4.769 4.174 4.174 4.174 0.000 -0.205 0.369 0.007 0.006 0.007 0.000 -0.369 0.431 13695 1232 1592 10665 23745 120542 2949Q14 2773 32944 $69.560 570.062 570.049 786.213 015.366 1.455a3 56.9432 1660.25 1659.31 570 570 570 786(N) 615(M) 1.46 56.9 1660 1660 QC Flag Legend M - Compound response manually integrated. ._ E':a;.Ct e_,o,,f Original l _niti,_ Dat_ 3M EnvironmentalLaboratory Page 86 of 276 Report E02-0443 . _ Tenn. River Valley Samples Data File: %\Etstarget%tart;et\che_\dudejr.i%l_)20629.b\DUDEOO7,).D 7.2- 6.96.6_ G.3; 6.0; 5,7; 5,4_ 5.i; 4.8" 4.6; 4.2: 3.9" 3.6" 3.33,0; 2.7 J ._, 2.4" 2.1=" i.8l.S" i.2" _! 0.9: 0,6- : \_Et starl_et\tart;et\chem\dudejr,i%D020_8. b\I)UIEO070.D .I Page 2 .... i .... J .... L .... i .... J .... I .... ! .... , .... i .... _ .... i .... i .... i .... I .... =.... i .... o .... i .... ' 0,5 t,0 1,5 2,0 a5 3,0 3,5 4,0 4,5 5,0 5,5 6,0 6,5 7,0 7,5 8,0 8,5 9,0 Hin i8 PFBS (299) 3.6- Ion 299,00 iv) 3.3" 3.0" 1 2.7" I 2.4: '1.6; 1.2" ,,4 _! 0.6:--__m._._ . i - i i . i 3.00 3.20 3.40 3._=0 3.80 20 PFHS (399) Ion 399.00 ; i.e. - _Ii __.6.-.4" II _. _.o: 08; O.G 3.40 3.60 3.80 H_n 4,00 4,20 ExacCt o_r:yJ:Or!_ina! Enitial Oat5 3M Environmental Laboratory Page 87 of 276 Report E02-0443 _llta File: \_Etstarl;et_tari;et\ohem_udejr.t_]>_20628.b_]_JDEO070.9 2J_ PFOA (413) 3.9- 3.3" 3.02.7" <_z.," v 2.,i _. 1,e: Ion 43.00, AJ f" 0,92 Min 22 FOS_(49S> Ion 498.00 3.6_ 3.3" ! 3.o- i z.4-' (I T )L/ i i 1l.s.-8: : i z.t" [/ O.SJ 0,6" 0.3 I I - - i # , * ", o'',. 4.40 4_.60 4,80 5.00 5.20 Hi" 23 PFOS (499> :i 7.0_ Ion 499.00 6.0- ..! ..o- ,:_ ' >- z.o" O O " l.O: m ,.o :1 ! i ........... ,-- 3.80 4.00 420 4.40 4.60 HSn .i i o_ Tenn. RiverValley Samples ..o Pa{;e 3 Exact Cc;_!,:,. , Initial Oat_ 3M EnvironmentalLaboratory Page 88 of 276 Report E02-0443 II . .. Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0076.D Report Date: 09-Dec-2002 13:08 Page 1 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0076.D Lab Smp Id: SL-3. LM-I-3 Inj Date : 29-JUN-2002 05:32 Operator : mla Inst ID: dudejr.i Smp Info Misc Info : Tenn. : River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstargetktarget\chem\dudej r. i\D020628, b\D020628, m Meth Date Cal Date : 09-Dec-2002 : 29-JUN-2002 13:01 00:48 dudejr.i Quant Type: ESTD Cal File: DUDE0050.D Als bottle : 42 Dil Factor: 1.00000 Integrator : Falcon Target Version: 4.12 Compound Suhlist : all.sub i Concentration Formula: Amt * DF * CpndVariable , Cpnd Variable Local Compound Variable iB .i 1 i.,i 'iIi' 1 Compounds 18 pFBS (299) 20 PF14S (399) 21 PFOA 22 FOSA 23 PFOS (413) {498) {499) QC Flag Legend M - Compound response OUANT SIG MASS 299 299 299 399 399 413 498 499 499 manually RT EXP RT DLT RT RESPONSE CDNCERTRAT3ONS ON- CObUMN FINAL (ng/mL) (ng/mL} 3.388 3.189 3,764 3.805 3.559 3.996 4.899 4.174 4.611 3.388 3.388 3.388 3.798 3.798 3.997 4.769 4.174 4.174 0.000 -0.199 0.376 0.007 -0.239 -0.001 0.130 0.000 0.437 37998 3724 1836 16875 3229 60835 78316 716542 12921 569.414 569.966 570.039 0.08359 786.407 0.95299 0.02433 1637.71 1659.94 569 570 S'_O 0.0836 786 0.gS31M} 0.0243(M) 1640 1660 integrated. I p , ExacCt opyofOdginaJ Date 3M Environmental Laboratory Page 89 of 276 Report E02-0443 . _ Tenn. River Valley Samples Data File: %%Etstar_et%tarl[et%chem%dudejP.t_)20628.b\])UDEOO76.D %_Etst_-Eet _tar cet %ch'm_dudre. i\_020(_28 b\DU[EOO7G]). 2,2" 2,i-: 2,01.9! t8! 3..7 i i,54 1,4- Pae 2 1.i: _1..0z-'- 0.9" O.B_. ::{ 0.7" 0.6- 0,5i i 0.44 :il o.3 t l 0.2{ " I-tl .... = .... 0,5 * .... i,O g .... i,5 I .... 2,0 = .... 2,5 I1 = .... 3,0 . tI I-- l = .... = .... ='" 3,5 4,0 4,5 Hin '= .... 5,0 t_l|| * .... 5,5 _ = .... 6,0 = .... 6.5 * .... , .... 7.0 7.5 , .... 8,0 , .... 8,5 * .... 9,0 28 PFBS(2_) 8,6= loin Z99k.0- 0mco ..z" II ". 4,40-!'. ::: _ 33,.$2-"" I/ II__ .t 2.4" _ II "/ 1,2! 0.8-__ 3,00 ., . , . . . ,. .. , 3,20 3.40 3,_0 3,80 . M_n . 20 PFHS(399) 3,2- Ion 399.0- 0_o 3.o- K :_' Z.S-:" ]; z.,'2"_ _ 2.2-_ v 1,6- > t.4_ ,'; 1.0" 0,8 -.': , , - . ,...i. 3.40 3,60 3,80 i 4,00 4.20 ExacCt opyofCri;_na! 3M Environmental Laborator_ Page 90 of 276 Report E02-0443 I IIII . _ Tenn. River Valley Samples Dat.a File: \\EEst.ar.get,%target",che_lude:lr. 21 PFOR (413) 66.0._." 5.5: 5.0" _ ,._" 4.0-': v 3.5i Zor_ 4t3.00(_ 2.5" >" 23..00:"__ 360 3.80 4.00 4.20 4.40 Htn 22 FOSR (498) Ion 49800 l%no2062a.b\DUDEO076]) :q l*'J- i 1.0-; 0.9_ 0.8_ I i oo.6.7_ =: 0,4 i 0.3-: . 0.2_ 0.'1!. I_ ..4...4.0......4..6..0... 4.80 Htn tJ 6.00 _.2 23 PFOS (499) i t.8" Ion 499.00 ., ! t.4" i i.2" o.e4 ). 0.6- o4 0,4" o.z-.: 16,_ - , 3.80 I * - - - , .... 4.00 420 H:lr_ , 4.40 = ,; I -J._l . B- 4.60 Pal;e 3 3M Environmental Laboratory Page 91 of 276 ReportE02-0443 II i . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0089.D Report Date: 09-Dec-2002 13:08 Page 1 3M Environmental Laboratory Data file : Lab Smp Id: Inj Date : Operator : Smp Info : Misc Info : Comment : Method : E02-0443 Tenn. River Valley Samples \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0089.D SL-3. LM-4-3 29-JUN-2002 07:55 mla Inst ID: dudejr.i Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. \\Etstarget\targetkchem\dudejr.i\D020628.b\D020628.m 20 Jun 02 Meth Date : 09-Dec-2002 Cal Date : 29-JUN-2002 Als bottle: 52 Dil Factor: 1.00000 13:01 dudejr.i 00:48 Quant .Type: ESTD Cal File: DUDE0050.D Integrator: Falcon Compound Sublist: all.sub :] Target Version: 4.12 Concentration Cpnd Variable Formula: Amt * DF * CpndVariable Local Compound Variable Compoun_ 18 PFBS (299) i; 20 P1="n_ (399} 21 PFOA (413) ' 22 F_A (498) .,_ 23 PFOS (499) _ QUANT SIG MASS 299 299 299 399 399 413 498 499 499 RT _P RT DLT RT RES_N_ _NCENTRAT ON- _LUMN (ng/mL) IONS FINAL (ng/mL) 3.395 3.190 3.753 3.805 3.552 4.003 4.769 4.174 4.605 3.385 3.388 3.385 3.798 3.798 3.99_ 4.769 4.174 4.174 0.007 -0.198 0.369 0.007 -0.246 0.006 0.000 0.000 0.431 12936 3732 1991 7393 2451 24746 64726 1029081 18761 569.610 569.966 570.033 786.298 786.427 815.313 1885.89 1627.64 1659.75 570 570 570 786 786 815(M} 1880 1630 1660 i QC Flag Legend M - Compound response manually integrated. 3M EnvironmentalLaboratory Page 92 of 276 Report E02-0443 . _ Tenn. River Valley Samples ]Data FL re: %_EtstaPget%t.t_l;;et%chem%dudejr, t%DO20C=_B,bH])U:DEOO89.][) Page 2 5.65.4-." 5.2" 5.0" 4.8- 4._" 4.4 -." 4.24.03.8, 3._" 3.4-_ 3.2" %_Etst4rll;e_,Ht_rll;et %x=heeq%dude r. L%DO2OE_8. bH]DU[EO0_. D 2.8_ i 32,.06-,_ >- 2.4" 2.2" 2.0, :i 1._" : :.4- i l.z- t .O,..Bo"_ 0.4- .... . .... , .... 0.5 , .... t.0 t8 _ <299) | .... i .... t.5 2.0 i .... 2.5 , .... 3.0 D .... 3.5 * ..* t .... 4,0 4.5 HLn | .... 5.0 , .... J .... 5.5 6,0 t .... 6.5 , .... 7,0 ; .... 7.5 _ .... BO . .... 8.B D .... 9.0 II Zon L:_9.0Q m i 3.6- 3.3- _g ,.; 3.0-" 'I z.7" z._: g d 0.92 0.6: .... 3.00 3.20 3.40 Him 20 PFFtS(3_=J> , ..... 3.GO 3.80 Ion 3_.00 m j i.3o- R ! _._.o" _ o.,4 ), 0.70-: 340 3.GO 3,80 4.00 4.2_ Htn ExacCt opoyfOrigina! o=o 3M Environmental Laboratory Page 93 of 276 Report E02-0443 Data File; _Etstarcet\tarcet\che_\dudeJr.i_J)O20628.b\DUDEOO89,D 21 PFOR(413) 4.2i 3.9" lon 413.00 o _" 3.3- 3.0,; P 2.7- v 2.4- > 1.8: i.5-: '1.2" 20o.91-:._. : , . . . , .......... 3.60 3.80 4.00 4.20 4.40 H_n 22 FOSA (498) Ion 498.00 ,.5-: 5.0-_ _i 4._ i 4.o_ , ; 35 i ' i / I _.o4: 0 i!: 3- 2.o-: 0.,4:'_ .... 4.40 '.,'_."'/I.t_,._.._h,! ..).. 4.60 4.80 5.00 5.20 Hin 23 PFOS(499) i 2.7- Ion 4,9..00 2.4" 2.t2 t.8" 1.5- '_ _ t.2; I ! Hin . _ Tenn. River Valley Samples PaEe 3 _,'.._itia! 3M Environmental Laboratory Page 94 of 276 a ReportE02-0443 . _ Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0102.D Report Date: 09-Dec-2002 13:08 Page 1 3M Environmental Laboratory Data file : Lab Smp Id: Inj Date : Operator : Smp Info : Misc Info : Comment : E02-0443 Tenn. River Valley Samples \\Etstarget\targetkchemkdudejr.i\D020628.b\DUDE0102.D SL-3. LM-7-2 29-JUN-2002 10:18 mla Inst ID: dudejr.i Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Method Meth Date Cal Date : \\Etstargetktargetkchem\dudejr.i\D020628.b\D020628.m : 09-Dec-2002 13:01 dudejr.l Quant Type: ESTD : 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle: 62 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub i Target Version: 4.12 i i Concentration Formula: Amt * DF * CpndVariable i Cpnd Variable Local Compound Variable i i ,_:,_ 1 ' Compounds 18 pFBS {299) 20 PFHS 21 PFOA (399} (413) 22 FOSA {498) 23 PFOS (499) QC Flag Legend M - Compound response QUANT SIG MASS 299 299 299 399 413 498 498 449999 RT EXP RT DLT RT RESPONSE CONCENTRATIONS 0N-COLUMN FINAL (ng/mL} (ng/mL) 3.388 3.176 3.757 3.799 3.997 4.769 4_441 3.388 3.38a 3.388 3.798 3.997 4.768 4.769 0.000 -0.212 0.369 0.001 0.000 0.000 -0.328 24706 1376 1023 9487 62864 23637 7"/9 569.154 570.057 570.C71 786.244 1.06124 1887.28 1888.05 569 570 570 786(M) 1.06 1890 1890 44..157958 44..117744 00..040214 90269720859 11663519..6403 11663600 manually integrated. i i "_actCo_ v__,. '0,/._;. ,j.-H.C.; 3M EnvironmentaLl aboratory Page 95 of 276 Report E02-0443 Tenn. River Valley Samples .o. Data File** \%Etstaeget;%_ar.get%t'J'_em_dudeJr'.i%]>)20628.b%gUDEO102.D 25-. 2.4: 23_ Z.Z-.: _%Et_at.ar'et\;=PEe%r 0hcH_\dudjeP. t \DO20C_2bB\.])UIEOI02.D 2.0_ 1.9_ 18_ 't .7_. 1.6-." t.5_ 1o4i 1.2. v 1.1-: Page 2 ,i "" t 0.8" ! 0.7" 1 !i 0 3-':. o.2_ I "...., .'---t-.--._-:----, _. , .... , .... .... , .... _.... 0 .... * .... * .... , - 0.5 10 1.8 20 2.5 3o0 3.5 4.0 45 5.0 5.5 6.0 6.5 7.0 7.5 80 8.5 9.0 HJn 18 PF'_3 299) _ 7.0_ Ion 299..00 6.s,' R 6.o" '; [ 15.5" I _.o,; ', 4.5-',. ", 3.5; , 2,0_ ,,'* _'*0i.. , . . , . . , , . ., . ., . 3.00 3.20 3,40 3.60 3.80 20 PFHS(399) ]on 3_..O0 '_ l"si Jl ";/_ t.2-: _._i t,0" ; _;-x t.4.-'i ]_t 0.7" .6 -i . 3.40 - ,. . , 3.60 3.80 Hin - i - - o 4.00 4.20 ExlctCopyof Original _ L,2ZC._J:_'-- Initial Date 3M Environmental Laboratory Page 96 of 276 Report E02-0443 Data File: _Etsta_et_ta_et\chem_dudejr.i%I_)2062a.b_DU_EOlO2.D 21 PFOA (413) 1.z" Ion 413.00 0.9! o.ai _ 0.76_i o.s" :" 0,4-." 0.24 8 ......... 3.60 3.90 4.00 H|n FOSA (498) Ion 498.00 J i. 4.20 4.40 7.06.0_ 5.0-: i4.! _ _ _.o-: 2.o- _ _ / / 44_ _6_ _e 5.00 5.20 23 PFOS (499) i 2.4. Ion 499.00 2.2_ .[ _..e-: , i.6" _ 1.0_ ; 0.6- t 0.4" ,_ 3._0 I 4.00 4.20 Hi_ II_-J 4.40 4.C_0 ,! . _ Tenn River Valley Samples Pace 3 ExacCt opy_f .Odgir,:,: Initial O_te 3M Environmental Laboratory Page 97 of 276 Report E02-0443 . _ Tenn. RiverValley Samples IIII Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0104.D Report Date: 09-Dec-2002 13:08 Page 1 3M Environmental Laboratory .,i E02-0443 Tenn. River Valley Samples Data file : \\Etstargetktarget\chem\dudejr.i\D020628.b\DUDE0104.D Lab Smp Id: SL-3. SM-I-I Inj Date : 29-JUN-2002 10:40 Operator Smp Info Misc Info Comment : mla : Tenn. : : River Valley Fish. Inst ID: dudejr.i Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Method : \\Etstarget\target\chem\dudejr.i\D020628.bkD020628.m Meth Date : 09-Dec-2002 Cal Date : 29-JUN-2002 Als bottle: 65 13:01 dudejr.i 00:48 Quant Type: ESTD Cal File: DUDE0050.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compounds 18 PFBS (299) i 20 PFHS (399) t .-',i 21 PFOA (41)) I 22 FOSA (49S) t 23 PFOS 14991 :i QUANT SIG MASS 299 299 299 399 399 399 413 498 499 499 RT EXP RT DLT RT RESPONSE CONCENTRATIONS ON -COLt_4N FINAL (ngJmI,) (ng]mL) 3.388 3.190 3.757 3.812 3.566 4.174 3.996 4.76g 4.174 4.605 3.368 3.388 3.368 3.798 3.798 3.798 3.997 4.769 4.174 4.174 0.000 -0.198 0.369 0,014 -0.232 0.376 "0.001 0.000 0.000 0.431 10955 2138 1256 _1252 5688 975 55673 41082 429027 15813 569,686 570.027 570.062 786.197 786.343 706.466 0.67774 1886.69 1646.86 1659.85 570 570 570 786 766 786 0.67B(M) 1890(M) 1650 1660 QC Flag Legend M - Compound response manually integrated. "t ExacCt opoyfOriginal , !n.it_al Date 3M EnvironmentalLaboratory Page 98 of 276 Report E02-0443 . .. Tenn. River Valley Samples Data File: %\EtstaPgetNt.srcatNchem_,dudejP.iNl>b2062g.bNDUDEO,O4.D Pace 2 5.65.45.2" _.04.84.6-" 4.4" 4.24.0: 3.8" 3.6-* 3.4" 3.2-*" N%Etst_r cat Xt arget %che_XckJdre. i_1_020628,b\DUIEOl04.D 32.08" 2.6>- 24" 2.2_ 2.0_. : Ii ; t.6_.4-_ i.2-_ .0" 0.e_ 0.6_ 0.4-: 0.2_ : ;.I I 0.5 t0 t.5 II IL_! I I s,A,0 I _ _..J_, 20 25 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 85 9.0 Htn t8 pFBS (299) _3_ 30 2.7: Ion 299.00 _ II _ f_ 'I "-;o- v.I J7 : o.,! 0.6"..,-,..,._,,-.L,._,.... . . , . . . , . . . , . 3.00 3.20 3.40 3.60 3.80 20 PFHS(3_> t.90- Ion 399.00 - i 1"'i h ._ '_1t _actCoOyof Or!,:;,n_: '.i _..,io' ',v I . 1t Y o o . . _ , _...o 3.40 3.60 3.80 4.00 4.ZO Hi, 3M Environmental Laboratory Page 99 of 276 Report E02-0443 . _ Tenn. River Valley Samples Data File: %%Etstar='4et\taret_chem%dudejr,i\_)20628.b_J_UDEOlO4.D 21 PFOR(413) 7.0_. ][on 4t3.. 6.5i " . 6.0 -." 5.5-:." 50 i 4.5 i i 40 _ v 3.51 >" 3.0 2.51 2,0! = D - - i _ - = 3.60 3.80 4.00 4.20 4.40 Hie 2Z FOSR (498) [o_rt 498_00 7.0- L 6.0" I 5.0-." : r 4.0" 2,0" T ,0-'. I i 4.40 4.60 4.8 5,00 5,20 Hin II 23 PFOS<499) Xon 499.00 ; i,0_ : O,9-:" , 0,8" 0.7" I 0.5" l _ o.4" i - i . m , - i - i 3,80 4,00 4,20 4,40 4,60 H_n 'i 'i Pace 3 ExactCopoy fOff#ins] _niUat O_,_e 3M Environmental Laboratory Page I00 of 276 Report E02-0443 . _ Tenn RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0105.D Report Date: 09-Dec-2002 13:08 Page 1 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstargetktargetkchemkdudejr.i\D020628.b\DUDE0105.D Lab Smp Id: SL-3. SM-I-2 Inj Date : 29-JUN-2002 10:51 Operator Smp Info Misc Info : mla : Tenn. : River Valley Fish. Inst ID: dudejr.i Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method Meth Date Cal Date : \\Etstargetktargetkchem\dudejr.i\D020628.b\D020628.m : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD : 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle: Dil Factor: 66 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compounds i.i_IiI.Iin_i_iIIiimi_I_I 18 PF_ (299) : i 20 P_S (399} i "_ _I pI_)A (413) 22 _SA 23 P_S (498) (499_ :_ QUANT SIG MASS _II. 299 299 299 399 3_ 399 413 498 499 499 RT _P RT DLT RT _Iii IIIiIii....i.l.= 3.3B0 3.388 0.000 3.182 3.964 3.82S 3.SS; 3.388 3.388 3.798 3._ 0.206 0.376 0.027 -0.2&_ 4.194 3.996 3.798 3.997 0.396 -0.001 RES_NSE ..=n..=. 11225 1896 1126 12780 S122 930 S2002 4.769 4 .i74 4.605 4.769 4.174 4.174 0.000 0.000 0.431 40143 4695_4 14246 _N_NTRATIONS _-_DUMN FIlL (n9/_) I.=_=._ (_/_) ....... 569.676 570 570.037 570 570.067 570 786.158 786 786.331 706 706.467 0.52474 786 0.525(N) 1886.72 1645.58 1659.89 1Bg0(M) 1640 1660 QC Flag Legend M - Compound response manually integrated. .+ E._acCto;:,o,_. Od_inal ! !p.!li_ 9at_ 3M EnvironmentalLaboratory Page 101 of 276 ReportE02-0443 II I III II II II . _ Tenn. RiverValley Samples ', ; i :',t Data File: \_Etstarcet%ter_et%chem\d_e_r,i_,D,_20628ob%DUDEOiOSoD Pa_e 2 _,%Etst_w'get%t _'l_et %he_%dt_ej r. i %]}020(:,28 b%DUIIEOto5.D 5,8_ 5,4" 5 2 -." _,0_. 4,,8- 46_ 4+4;, 42-.: 4.0_ 3o8_ 36" 3.43.2-.: 3.o_ _._ _" 2.64 _" 2.4" 2.2" lO-: i._- i.4_: i.2" _.o-_ o.8" 0.4;" 0.4_. 0.2-' :t..._. I _ --'_t..I.I._ ...... =.... 0.5 l.O _ .... i.5 I .... 2.0 ' .... 2.5 IIll.... ILl) ' .... 3.0 3.5 IlSl*._....ll__ Ot't 4.0 4.5 "'! .... 5.0 ' .... 8.5 ' .... 6.0 I .... 5.5 O.... 7.0 I .... 7.5 ' .... e,o _ .... 8.5 ''_'" 9.0 18 PF3S (299) 3._-" 3.3-: 3.0" 27_ Ion L>_).O0 ,,; _- _.e" '; ,J 0.9 i._" i3;" i);" i._" ig ffl, 20 PFNS (3_) Ion 399 O0 : _ . i _'_" _ I\"A ,.4" / I= lli too 3.40 3.0 3.80 4.00 4,20 ' l H_ n ::,:_C,,;uL;'vo_Original $ 3M EnvironmentalLaboratory Parle 102 of 276 Report E02-0443 :_ 5t _ i :i. l i Data File: _\Etstart;et_target_chem\dudejr.i_l>>20628.b_)UDEOi05.0 ;H PFOA (413) Ion 4t3.00 5.6: _. 4.E 4.1 _ 3.( x 3.; 2,4 2.< 4,_ 3.60 3.80 4.00 420 4.40 22 FOSA (498> Ion 498.00 .i / 7.o- S.O_ 5.0" 43..0o"i z.o- 1.o" i,,:__ _ 4.40 , ,_? 4.60 4.8,> Hin 23 PFOS (499) ) 5.f_.o 5.20 [o_ 499.00 2.0" ,,4 0.8- 0.7 i 0o.9."s" IT 0.2" o._ i 3.80 _j i - i . i 4.00 4.20 4.40 Hin . '_,; ,_ , , 4.60 i ' ._ Tenn. River Valley Samples Page 3 ExacCt opoyfOrigina! Init/al Date 3M Environmental Laboratory Page 103 of 276 Report E02-0443 n . _ Tenn.RiverValley Samples i i III Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0108.D Report Date: 09-Dec-2002 13:08 Page ! 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr. i\D020628 .b\DUDE0108 .D Lab Smp Id: SL-3. SM-I-3 Inj Date : 29-JUN-2002 i1:25 Operator Smp Info Misc Info : mla : Tenn. : River Valley Fish. Inst ID: dudejr.i Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstarget\target\chemkdudejr. iiD020628.b\D020628 .m Meth Date Cal Date 09-Dec-2002 : 29-JUN-2002 13:01 dudejr.i 00:48 Quant Type: ESTD Cal File: DUDE0050.D Als bottle: Dil Factor: 67 1.00000 Integrator : Falcon Target Version : 4.12 Compound Sublist : all. sub E Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable J ; i 1 i = ; i:i ,_ Compounds 18 PFBS (299) 20 PFI_S (399} 21 PFOA {415) 22 FOSA 23 PPOS (498) (499) QUANT SIG MASS 299 299 299 399 413 498 499 499 RT EXP RT DLT RT RESPONSE CONCENTRATIONS ON- COLUMN FINAL (ng/mL} (ng/mL) 3.368 3.183 3.784 3.798 3.996 4.762 4.134 4.598 3.388 3.388 3.388 3.798 3.997 4.769 4.174 4.174 0.000 -0.205 0.376 0.000 -0.001 -0.007 0.000 0.424 16091 2727 1508 13195 54265 44388 450983 15684 569.488 570.005 570.049 786.147 0.60270 1886.57 1645.91 1659.85 569 570 570 786(M) 0.803(M) 1890(M) 1640 1660 QC Flag Legend M - Compound response manually integrated. ExacCt opyof Ori;_na! /-.w.(__/.aZm./z>,- :'i _i_ Oate 3M EnvironmentalLaboratory Page 104of 276 Report E02-0443 .. _ Tenn. River Valley Samples ]Data File: %_EtstaP[etNtaPcet_cJ_m_dudejP.i\l_)20628.bN_JDEOlOS.D Pace 2 5,8_ 5.6_ 5.4:. s.2-: B.O" 4.8_ %%Est tJccet\tac_et%ch_m_lvll ir. i%DO20_2,Bb_J_UIEO$O.]_D 4.4- 4.2_ 4.0- 3.8! 3.6-." 3.4-." 3.2-.: ,_ 3.0- 2..- v 2.6" _- 2,4i 2.2" 2.0_ i _LG- : :L.4_ l.Z" '._ 0.8** 0.6" O.4_ 0.2_ :1.1.1.;.I, 0.5 1.0 t,5 III I_1 II 11#_11_11 I 2.0 2.5 3,0 35 4.0 4.5 5.0 5.5 6,0 6.5 7.0 75 8.0 8,5 9.0 H_,_ 28 PF]_S(299) i Ion L>J_,O0 :2! -." !*i ! Jl ,Y -.-.:_ 3.00 ..... ............ 3.20 3.40 3.60 3.80 M_n Ion 399.<)(> 3.2: A- ' _-i I} ,_ 2.4 " 2.0-: v :_.8- "t.4" I.<_ ._,_._,_.3.,8.0 ..4..00..4..2.0 .. Hjn E_acCto:Jry,.Or!_n,! !nJtJa! :;)_5,-'" 3M Environmental Laboratory Page 105 of 276 Report E02-0443 Data File; %_EtstaPcet\tarCet\ohe#_dudejr,i%DO20628.b\DUI)EOiOS.D 2i PFOA (413) G,4_ 6.0" Ion 413.00 m 4.E _,. 43.1 >- 3; 2.4 2.,q 2. 3,60 3,80 4,00 4,ZO 4,40 Hln F_A 498) tort 498.00 80- 7.0-" 6.,0_ "'0i 4.o_ 2.0" !,.-- -- I _/_.-,.,--._ I,/ " * " * * * - * =- t 4,40 4,60 4.80 5,00 5,20 Hln 23 PFOS (499) i.i= : 1.0_ Ion 499,.00m 14 * 0.9" ! '8i i 0.7- ; v 0.4" >" 0.3_ , 0.2" m o.i-:: / i ." 3.80 4.00 4.20 4,40 4.60 Nin : ,.i f, . _ Tenn. River Valley Samples Pa_e 3 ExacCt opy_ Origina} _il_ Date 3M Environmental Laboratory Page 106 of 276 ReportE02-0443 . ._ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0089.D Report Date: 27-Aug-2002 10:06 Page 1 3M Environmental Laboratory 802-0443, Tenn. River Valley Samples Data file : \\Etstarget\targetkchem\dudejr.i\D020629.b\DUDE0089.D Lab Smp Id: SL-1. WB-I Inj Date : 01-JUL-2002 04:25 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Misc Info : Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m Meth Date : 27-Aug-2002 Cal Date : 30-JUN-2002 Als bottle: 47 09:59 dudejr.i 22:46 Quant Type: ESTD Cal File: DUDE0058.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compc_nds m=..n==--==-- 18 pFBS s _m._=.n== 4299) _ _n.= 20 pFMS 21 pFOA 22 FOSA (3998 44138 (4988 23 _WO5 {4998 ,! ! QUANT SIG MASS =m.m 299 299 299 399 413 498 499 499 RT EXP RT m=_= .==m==mR 3.313 2.944 3.381 3.381 3.163 3.381 3.798 3.792 4.004 3.990 4.776 4.756 4.188 4.148 4.60S 4.169 DLT RT m===.=== -0.068 -0.437 -0.218 0.00S 0.014 0.020 0,020 0.637 RESpONSB =.. _ ==== 32577 478 2981 8170 10932 7648 96923 22825 CONCRHTRATIONS ON-COLUMN PZNAL (ng/mL) ===inn= 1223.22 1224.$4 1224.39 0.16435 819.144 2744.00 1274.9_ _n /mL ) t.=..n. 1220 1220 1220 0.164 819 2740 1270 1277.09 1280 I 3M EnvironmentalLaboratory Page 107 of 276 Report E02-0443 Tenn. River Valley Samples 3ata File: ',.\Etstar'get_.target_chem%dudejr.f,_.DO20<o29.b_.X)UDEOOBg.3 2.4_ 2.3i 2.22.12.0_ 1.9" 1.8i 1.7t,6:. 1,5-: _Et st aPge t \t, arget \cheM\dude r. i _3020629 .b%])U_EO08?. B _ '-_i ..>" toli 1.- !t 0.,4 ,8_ 0.7_ O,G-: It Page 2 .3 ] 2 i t .... t .... i .... t .... i .... ! .... i .... i .... _ .... t .... .... _ .... 0,5 1,0 1o5 2,0 2,5 3,0 3,5 4,0 4,5 6,0 5,5 6,0 6,5 7.0 7,5 8,0 8,5 9,0 H;n 18 PF3S (299) / 3,: 3._" I 3.0" j 1 /,, 2._" I /P 2,4: t _I / _ =.o _I }, , t.2;_ /\.t I "_._ _.2_ _.4_ _._ / ....... Hln 20 PR-IS <399> _.8_ I 2.0-- tl t,9" II____..4-2__ Hr_ I_1-o II .6" .4 i I 3.40 3.60| 3.80 4.00 4.20 ExacCt o:];:,:,:.3;-::;;:., Lqltial,0_,-. 3M Environmental Laboratory Page 108 of 276 Report E02-0443 _a_a File: \\Etstargeb%targeb%htcq_udejr. 21 PFOA (413) 2.8_ 2._- 2.4_ 2.2" z'o! Ion 4t3.00 _- o _1 _ _1 II l_020629.b_U_EO089._ =.o-= / "i. 22 FOSA (498) Ion 498.00 i.6-" g_ 0.8: _" 0.6: t i , i | i 4.40 400 4.80 5.0(3 820 lltr_ 23 PFOS (4993 1.8- _..6" Ion 499.00 .2:o 4! i 0i..08-_ :I :,. 0.6" : 0.4! 0.2-" : ...... 3.80 I, ," / .... -"/_, 4.00 4o_'0 4.40 460 Htn - _ Tenn. River Valley Samples Patge 3 ExacCt o)?o_Ori.3ina] 3M Environmental Laboratory Repod E02-0443 II - - Tenn. R_er Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0127.D Report Date: 27-Aug-2002 10:07 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstargetktargetkchemkdudejr.i\D020629.b\DUDE0127.D Lab Smp Id: SL-2. WB-I Inj Date : 01-JUL-2002 11:23 Operator : mla Inst ID: dudejr.i Smp Info Misc Info Comment : Tenn. : : River Valley Fish. Prep-17 Jun 02. CMC/MLA. Method Meth Date Cal Date : \\Etstargetktarget\chemkdudejr.ikD020629.bkD020629.m : 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD : 30-JUN-2002 22:46 Cal File: DUDE0058.D Als bottle: Dil Factor: 76 1.00000 20 Jun 03 i Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub i Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Ccxspo%uldm 18 PPBS (299) 20 pFH8 (399) 21 PPOA (413) 22 708A (498) I 23 pPOa {459) I ! QUANT SIG MASS 299 299 199 399 413 498 499 499 RT EXP RT DLT RT RBSPONSB CONCENTRATION8 OH- COI23MH FINAL (ng/mL) (ng/mL) 3.319 3.178 3.791 3.982 3.996 4.776 4,181 4.598 3.381 3.3Sl 3.?92 3.792 3.990 4.756 4,168 4.168 -0.062 -0.20S -O.001 0.190 0.006 0.020 0,020 0.430 21873 3704 3814 1921 12881 3433 86874 12403 1223.32 1224o]5 0.03478 797.168 819.015 2744.18 127S.20 1277.40 1220 1220 0.0348 797 819 2740 1280 2280 :I ,::':ac_C.,_., _, Original '; ;ni_a.I O_te 3M Environmentall_bor_forv Report E02-0443 I - - Tenn. RiverValley Samples Data File: %_Ebstar=et%t_et_:heM_udejP,i%DO20629.b\DUDEO127.D 2.8! a7_ Z.6_ 2.5_ 2 4-:. 2.3" 2.2-." 21: 20_ 19_ 1.8! 1.7 i i, 5-." i t,6... i.3- i2_ 4 i.i_ iO" 0o9" \\Etst_'Ket_t_'et_chem\dudej r. i _])020629. b_)UDEO127.D Pal;e 2 05" o," _ 03i ' "' ' ;_'" i_;'" i_'" 11;'"ii.'" _1_'"i_5""ili'" _;.'" _; ""5;_'"_3""i15""_,1";"_1_'"i31;"'i31_' ' _i; """ Hi.n 18 PF_S (2_) 4.2" I(_t 299._0 I 3.s_ 3.3: 2.4: > 1.8" i.5- t.20.9- H|rt ,, 20 PFHS 399) Ion 399.00 N ' i.oo_ l o.,oj I_l( I= o0._o_ i, 340 3.60 y3.80 400 4.20 H_n W'(,_:L;> =, _4,,-z_ _;g,o/o__ .... 3M Environmental Laboratory m_,_.. _ _,_'_ Report E02-0443 3ata File: %%Etst_get_t_egetXche_%dudejri_,OO20629bXOUDEO127,D 21 PFO_ (413) 3.s 3.3.! 3.0-' 2.72.4: Ion 4t3.00r_ r_ v 1.5_ 1.2:. 00.96"i.,.,.,..,._._...,.LJ i =* | - i - , - 3.60 3e0 4,00 4.20 4.40 Hin 22 FOS_ (498) I/ | . P 4,40 4,GO Hin *, 4.80 . m. i 5.00 5.20 23 PFOS (499) 1.6" 5 I(_I 499.00 m 1.4-" T t _.2 '! o.a:. m v o,=,: i _- o.4_ : 0.2_ :J_ i t-._o.: ": Il I * - i i - i *I 3,80 400 4.L:'O 4,40 460 mn. - - Tenn River Valley Samples _ PaTe 3 @ Report E02-0443 - - Tenn. RiverValley Samples Data File: DUDE0089.D Report Date: 27-Aug-2002 11:06 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE0089.D Lab Smp Id: EL-3. WB-I Inj Date : 03-JUL-2002 07:02 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Misc Info Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Con_nent : Method : \\Etstarget\targetkchemkdudejr.i\D020702(D20702).b\D020702.m Meth Date : 27-Aug-2002 II:01 dudejr.i Quant Type: ESTD Cal Date : 03-JUL-2002 01:21 Cal File: DUDE0058.D AIs bottle: 72 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable CoBpoundm mlmmmm.mmmmmmmnmmRm_iBmmm 10 PI=B8 (299) 20 PPH n (399) '_ 21 PFOA (413) ! 22 FOSA (49E) _i 23 PFO8 (499) DtlAHT slo MASS mmms 299 2)9 299 399 299 43,2 49B 449999 RT _XP RT mmmn m_mmm.mm 3.321; 3.181 3.777 3.387 3.3S7 3.387 3.B2S 3.$45 3.7J1 3.791 4.010 4.803 "t.gt9 4.740 DLT RT m_mmum_m -0.061 -0.204 0.390 0.034 -0.246 0.011 O.OSS R_PONSE mmmmm.=m 2S'a2? 3221; 498 7B77 937 14443 5535 44.,159941 44..11_17;7 00.,403247 l=l2t24943S7 CO_T2ONS OB -COLOR (ng/mr.} mm_.m.m 1219.58 _.120.47 1220,5B 0.21;845 0.12420 "@S5.103 2854.35 11332243..:042 pINKL (ng/mL) ==mummm 1220 1210 1220 0.2S8 0.124 "/gS(N) 28S0(M) 11332200 QC Flag Legend M - Compound response manually integrated. : _._acCtopy(.O,rfi..'l:n:< 3M EnvironmentalLaboratory Paoe 113 of _'76 Report E02-0443 "- Tenn. River Valley Samples ,]1 Report E02-0443 Data File: %%Et,starget%t_get_he_Judejr.L%9020702(])20702).b%gUnEOO89.D 2 PF(3_ (413) 26-: 2.4_ 2.2_ 2.0-" [o_ 4_.3 .GO o _. 4-." v _.2- _.o- 3.60 3.80 4.00 4.20 4.40 Htn 22 FO_I io8_ (498) |on 498..00 P_ ;, *.z" o :. o.g" 06: 0o4"__ 4.40 I" 4,GO 4.90 Htr_ 2;3 PFOS_.,_aj_ _..2_ ;on 49900 500 5.20 ; 10_ 094 084 06-_ 015" 0.4-'. 03 i 0.2_ ,) HIn - - Tenn River Valley Samples Pal;e 3 3M Environmenta} Labor_fr, n, _ ........... ReportE02-0443 . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0064.D Report Date: 27-Aug-2002 I0:05 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley SamDles Data file : \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0064.D Lab Smp Id: SL-I. C-I-3 Inj Date : 30-JUN-2002 Operator : mla 23:51 Inst ID: dudejr.i ; Smp Info : Te_n. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info : Comment : Method : \\Etstargetktargetkchemkdudejr.i\D020629.bkD020629.m Meth Date : 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD Cal Date : 30-JUN-2002 22:46 Cal File: DUDE0058.D Als bottle: 28 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 L Concentration Formula: Amt * DF * Cpnd_ariable i Cpnd Variable Local Compound Variable CompoundJ m=mBm.m===E=l_slJnnm.=g'Jm In PFBS (299) '20 PPH.q (399} 21 PL:'OA (413) 22 POBA (490) :; 23 _WO_ 6499} u QUAHT 826 MASS =..g 299 299 299 399 413 49i 499 49_ 499 RT m.l_ 3.306 3,176 EXP RT _m.==B_ 3.381 3.311 3.751 3.798 2.997 4.7513 3.381 3.792 3.990 4.756 4.17 m: 4.434 4.605 4.166 4.106 4.168 DLT RT m=..m.== 0,007 -0.20S 0.370 0.006 0.00? 0.000 0.00? IJ.2,6 0.437 RESPONSE ==g==_=m _2710 3939 2r, s r. 7182 23937 _L401325 400664 5770 16925 CONC_HTRA.T2ONS ON- COLUHN FINAL lng/mI_) Bm==m_= 1223.64 1224.34 1224.42 0.1362_; 0,38259 r-.203BI 10.0262 2277.60 1277.27 (ng/uL) _s.==m= 1220 1220 1220 0.1366N) 0.302(N} S.206NJ 10.0 1200 1200 QC Flag Legend M - Compound response manually integrated. i ,i 3M EnvironmentalLaboratory Paae 116 of 276 Report E02-0443 -- Tenn. River Valley Samples 9ata File: %%Etstaret%t_ret%cher_\dudejr.t%OO20629.b\gU]OEOO64.D Pe 2 7.26.9" 6.6" 6.36.0-_ 5.7" 15.4" 5.1- 4.84.54.2-' 3.9_ %%Et.sforcer %tar Cet%che_\dude r. i %902029. b_UDEO064 oD 33.3."6" > 3.0, 2.7-" 2.4_ 2.11.8" 1.5" 1.2, 0.9" 0.6, 0.3, III II IllJL.f_tl I I _II II "'" o'5" i'.o' "].'._' "],'o""V._'"_'.o' ' _:_" 4'.,";";_'.",_"5",";"5:_'"_,'."_';6:_'"_" Hip '18 PF_3 (299) "-_5' "8%'"8;_'",:,_""' , Ion 299.00 3.3- /I RI : _.o" _l ";/ ; _.i: " /I I.v 20 PFHS (399) 2.8z._;._ z.4. _'_ 2.0-" Ion 399.00o. ' _, P. ,,,; _. _..41.2 1.0-_ 0.8:. _,.,_. _'_' _.'_"_,.'_' _,.'_ H_.n _:_CZ C_3y ,,.",,".,!._',i. -. ZL_L_./_./<o/o.z_... Report E02-0443 _at.a File: %%EEstar=et\taPge_\chem\dudejr.i_J)O20629.b\gUDEO064.9 2.1. PFOA (413) 4.e4._" 4.23.93,6: Ion 4.t.3, OOf.,. _, ,_ 33..30"_ 24" _..8-: 2.7"______ 1.5-'. &.2-" , 3.60 , , . . . , .. . , 3.80 4.00 4.20 440 Hin 22 FOSA (496) Ion 498.00 5.0 -'.' = 4.0" q_ 3.0" 2.0" :" :L.5; t.0 i 0 "8 _h,,.,,,_.i....._..,,_ J.-, 4.40 4._0 Hin =4.80 .. = ,, i 500 6.20 23 PFOS (479) I ][on _L.O_ 0.1_-: o.7_ 0.15- >" 0.3-'.: 0.20.1-.: 0o4 -'._ 3,80 4.00 4.20 4.40 4.60 Htn -- Tenn River Valley Samples Page 3 _-_XaCCot;;_:,:..,;_.::._ _itjat O_i:- 3M Environmental Laboratory Repod E02-0443 - - Tenn. RiverValk_ySamples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0065.D Report Date: 27-Aug-2002 10:05 Page 1 3M Environmental Laboratory Data file E02-0443, Tenn. River Valley Samples : \\Etstarget\target\chem\dudejr.i\DO20629.b\DUDE0065.D Lab Smp Id: SL-I. C-2-I Inj Date : 01-JUL-2002 00:02 Operator : mla Inst ID: dudejr.i Smp Info Misc Info : Tenn. River Valley : Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method Meth Date Cal Date : \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m : 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD : 30-JUN-2002 22:46 Cal File: DUDE0058.D Als bottle: Dil Factor: 29 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compounds m=======_=mBi=.lm=_usa_. 15 PFBS (299) ! 20 pFHS (399) i_ 21 PFOA 22 POSA (413) (498) 1 23 PPO8 (499) i QUANT SIG MASS _=sw 299 295 299 399 399 399 413 49| 499 499 499 RT _=um EXP RT i=w=i.a= 3.208 3.381 3.169 3.751 3.798 3.402 3.381 1.301 3.792 3.792 3.539 3.997 4.753 4.175 3.792 3.792 3.990 4.756 4.168 4.168 4.605 4.169 DLT RT _==i=lwm 0.007 -0.212 0.370 0,006 -0.390 -0.253 0.007 0.007 0.007 -0.376 0.437 RESPONSE _= = iDIRn 13624 2006 1621 10531 100& 2533 267?$ 122104 4?2057 2335 21371 CONCRNTRATIONS ON- COLUMN FZNAL (ng/mL) =l=ma=. (ng/mL) B==.==i 2223.79 1224.40 1224.47 0.21151 797.194 0.00404 0.54153 4.44736 9.?_111 1277.70 1277.14 1220 1220 1220 0.232 797 0.00404 0.542(M) 4.45 9.76 3250 1280 QC Flag Legend M - Compound response manually integrated. , "i i_iIi_I Dat:; 3M EnvironmentalLaboratory D_ i_o _ 07_ Report E02-0443 . _ Tenn River Valley Samples ,I ; I _! ])ata File: %\Etstarl;et_t_ret%chem%dudejr.i\DOZO629.b_])UDEOOG5.D B.2" 5.04.8" 46i 4.4' 4.24.0 _ 3.83.&3.4" 3.2' 3.0" \'_t $'c.ar.Ee_%t ar.K et %che_%dude r-. i \_202_3. b'_UDEo085. D Pal;e 2 2.6i 2Z.84-" >" 2.2- 2.0_ t.e- :_.,6-: _.,4=. 1o2_ _.o_ 0.8- 0.6- o,_ II 02" !,, u_t,I : t _ LjL, , J_L. It, ,, o's i.o _'_ z'o z:5 _.o _.s 4:o ,.s S:o ,:_ 6:o _:5 Y.o _.. b:o e.5 9"o Hin 18 PF3S (L:_9) 42" 3.9; , 3.G_ 3.3-" Ion 2_9.00 . ,,'4 _ 2.4- _ J ] :,. 2.i- r_ ) i 3,0-' 2 i 3.00 3.20 3.40 3.80 3.80 Hi. ! 2o PFHS (399) .; 2.e_ _ z.6_ ,; 24 I z.z- Ip, z.o" ]on 339,00o_ >- i.4: m , j _..z- 1.o, 3.40 3.60 3.80 4.00 4.20 _vaC/Cc_;_ 0 _'2,!gJn;.lj !nI_ Oa_ 3M Environmental Laboratory p=_,, _on _ :_7_ Report E02-0443 Data File: %%Etstarget\t_get%cheM\dudejr. PFO_ (413) 6.0: s.z_ 4.4: 4.0! 3.6-" _ _.z- " 2.8_ Ion 413.00 Kg II )" 42.84-._: .L I/ ," i-.-J 3.60 - m m* - i 3,80 4.00 Htn 4.20 4.40 FOSR (498) i_J)O20629.b\gUDEOO65.D ,_ e' i ' 7.0" ; 6.0_ : ; 5.0- Ion 498.O0 / : " r,. _ 4.0-." _ 3.0._ i.O. i_ -- mt . , , , - , - i .... 4.40 4.60 4.80 5.O0 5.20 23 PFOS (499) Ion 499.00 m 8._ 7.0! 5.{ "_ _I ! /\ , 3.',,.'_,i_._,4_._,.,_ -- Tenn. River Valley Samples P_ge 3 _.rljtjaJ Oate Report E02-0443 I I . _ Tenn. RiverValley Samples I I Data File: \\Etstarget\tar_et\chem\dudejr.i\D020629.b\DUDE0071.D Report Date: 27-Aug-2002 10:05 Page 1 3M Environmental Laboratory E02-0443, Ten n . River Valley Samples Data file : \\Etstargetktarget\chemkdudejr.i\D020629.b\DUDE0071.D Lab Smp Id: SL-I. C-3-2 Inj Date : 01-JUL-2002 01:08 Operator Smp Info Misc Info Comment : mla : Tenn. : : River Valley Fish. Inst ID: dudejr.i Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Method : \\Etstargetktargetkchem\dudejr.ikD020629.b\D020629.m Meth Date : 27-Aug-2002 Cal Date : 30-JUN-2002 Als bottle: 34 09:59 dudejr.i 22:46 Quant Type: ESTD Cal File: DUDE0058.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 [ : Concentration Formula: Amt * DF * CpndVariable ; Cpnd Variable Local Compound Variable _[_undm =M==m=nmm.mmsl.=mm_l.am==_ 18 PFB_ (299) i ,a ! 20 PPHS (399) i 21 pPOA (413) I 22 )'O.SA (40)8} }_ 23 PPOS (499) l : QC Flag Legend DUANT 5IQ HUB .-_= 299 _99 299 399 413 4.98 498 49J 499 RT m.ma 3.38| 3.17G 3.750 3.79| 3.997 4.762 EXP RT nl_====m 3.381 .'a_l 3.381 3.792 3.9_0 4.756 DLT RT _=m.==_= 0.007 -0,20S 0.360 0.001[ 0.007 0.006 RESPONSB I===_=m= 1S305 2054 2430 12488 20288 18S959 5.00_ 4.174 4.605 . 75 4.188 4.1Sa 0.2S "t 0,001; 0.437 9781 742237 2017E CONC_NTRATI ONS ON-CO_S PINAL {ng/mL) .=n..== 122].89 1224,45 2224.48 0.28719 0._7834 7.07763 (ng/m5) ==.=m.. 1220 ",220 1220 0.287(H) 0.178(H) 7.00 2"243. %2 17.9441 1277.17 2740 I?.9 1280 M - Compound response manually integrated. iii 3M EnvironmentalLaboratory Page 122 of276 Report E02-0443 ._ Tenn. River VaLley Samples Data File: %\Etst_u_[et%_=(et%chem\dude_r.i%OO206_.b\_UOEOO71oD 30 i 3,6_ 3.4-: 3.2! 3.0-" 2.82.6: 2.42.2- ,_ z.o-: _o8: \_ t st ,_r_e t\ t.ar_ _._chlm_cle r. i\D020(>29, b\_0071. ]D Pst;e 2 1.4. _i "i ' i ii _ ; 1." 0.6" 0.4: II 0.2-' I II II II IO I IJ I_ l_,bl .... a .... ,.... , .... , .... i.... J- -.-_n.... * .... e.... _.... , .... p .... =.... * .... i.... o.... m .... | .... 0,5 1,0 _.,5 2,0 2,5 3,0 3,5 4,0 4,5 5.0 5+5 6,0 6+5 7,0 7,5 8,0 8,5 J.O 18 PFBS (299) ;on Lx_+O0 4,40_ I_1 3+_-: _ 3.z-: 2.8- /t z.o_ I t.6-" _,2-_ z.4,_ _:_- o o , -. o... o. 3.00 3,2_h3.40 3.60 3.80 20 PFHS (3_) "!; _3.'0:;_': ! I^ 2o;'! zo,_.oo, 2.t*" 1.8_ 1.5-; 1.2" .9 o._: 3.4__.'_"3.'_ _'_ ;.'_ ., H_n .... _ili_! _: EXaCCt{_,:;:_: _ _ 3M Environmental Laboratory Page 123 of 276 Report E02-0443 " - Tenn. River Valley Samples Da_ File_ _E_star_eb_targetSchem_jr.l\DO20_29.b_DUDEOO71.D 21 PFOA (413) 1on 413, OOr_ 4.5i 4.0i 3.5_ 3.0i > z.5_ I t.5" 5_.L00._-'." z.oi _.6_",_.8,;",_._",;.zG",L4G I H|n 22 FOS_ (498) I_ 49B,00 _..6! 1,4" "l v ,_ )- 0,6- " _ _ 0.2" u; i_ i ,,) - , o i |- , i . 4.40 4.60 4.80 5.00 5.20 Hin 23 PFOS(499) 1o6_ ;on 499.00 i 1.2- o.4_ 0.2. 3.80 _r I I 4.00 4.20 4,40 4,60 HJr_ Pal:e ReportE02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0076.D Report Date: 27-Aug-2002 i0:06 Page 1 3M Environmental Laboratory Data file 602-0443, Tenn. River Valley Samples : \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0076.D Lab Smp Id: SL-I. C-4-2 Inj Date : 01-JUL-2002 02:03 Operator Smp Info Misc Info : mla : Tenn. : River Valley Fish. Inst ID: dudejr.i Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstarget\targetkchemkdudejr.ikD020629.bkD020629.m Meth Date : 27-Aug-2002 Cal Date : 30-JUN-2002 Als bottle: 37 09:59 22:46 dudejr.i Quant Type: ESTD Cal File: DUDE0058.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 ; Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable i i ! Compounds .=mmlm=.w=m_=g.m=B=_mm=m= 18 PPB,g (299) , ; 20 pitHS (399) 2"1 PFOA (413) b 22 ]_'O_ (498) 23 pPOG (491)) i QUAI4T SI[G MASS m=== 299 299 299 399 413 498 499 499 499 499 RT _= 3.3B1 3.224 3.750 3.792 3.997 EXP RT =..==m=_ 3.381 3.361 3.301 3.792 3.990 Dr,T RT a_====_= 0.000 -0.157 0.369 0.000 0.007 R_SPONSB ==m_==== 13243 2813 629 5712 11767 4.749 4.174 3.785 4.434 4 ._;OS 4.766 4.168 4,168 4o168 4 .1Gm 0.013 0.006 -0.383 0.264 O. _&3_' 103527 684549 511; 11460 3DG29 CONCENTRATIONS ON- COIA_MH (ng/mL) =====.. 1223.81 1224.40 1224.53 FINAL (ng/mL) .Js_=m= 1220 1220 1220 0.09444 819.097 0.0944(M) I19(H) 3.G7245 16.1878 1277.75 1277.43 12"Y7.1S 3.67 11;.2 1260 1280 I_80 QC Flag Legend M - Compound response manually integrated. 3M EnvironmentalLaboratory Page 125 of 276 Report E02-0443 , _ Tenn. River Valley Samples l)ata Fi]e: \_ELst,arl:et_,t,aPcet_ch_m_dudejr.iM)O20629.b_gU_EOO76]J _._.Est,t,arl;et,\t, aPet,_.che_lude r. i_.9020_9.b%]_JDEO076.9 2.3" 2.2" 2.t i 2.0" 2.9 i 1.81.7" 1.6" PaEe 2 1.3" _ _'_! 0,8" 0,7-:." 0.5-_ _! 0., '._,i .... _ ..... .1. .** .... * .... , i ., .... i .... i .... i .... i .... 0.5 1.0 15 2.0 2.5 3,0 3,5 40 4.5 5.0 5.5 6o0 6.5 7.0 7.5 8,0 8.5 =J.O H|n 18 PFBS(299) Ion 299.% 3.6: r_ 33-" 7] i 3.0: i 2,7: :. ,..- .;f : '- Hf_ I 1.2-: OJ)'_ * ..| .*. p* * , - * i 3,00 3.20 3.40 3.60 3.80 HI_ 20 PFHS (3_) :! 2.2- _; :! 2.o! I 2.4- : _, 1.r,z 1.4,_ !>" 1.2-: 0.8 i .j. 3,40 . , . . . D. 3.60 3.80 Hin . . ,, 4.00 . t 4.20 i.-.'xaC,_,.:.,: _ I'll!ti_ _ . 3M Environmental Laboratory PaQe 126 of 276 Report E02-0443 Tenn. River Valley Samples -w _ata File: \_E_s_;arl;e_\aPge_\ch_q\dudejr.L\9020629.b%gU]OEOO76,D 21 PFOR(43) Zon 4_.3O0 3,6-.' 3O tt _ _ 2.7 ._ 2,4 :" i.8 'eL,5. dL,2_ 0,9". H;n 22 FOSA(498) Ion 498,00 70-: 6,0" 5,0- i 4.o:: >" 2,0" 1,0-' _.o': _ _ ! :_'. i .I. , . . . , . . . , .I.. . 4,40 4,60 4,80 5,00 5,20 Hin 23 PFOS(499) Ion 49900 ,q. d.,4- _i _.o" i " 02-: * I" :,,,J I I _ I I /J"_J * - ' I I "D" I ' 3,80 400 4,20 440 4,60 H_n t ,..i Pae 3 ExactCo;j.........,.-_..,:":.".: Inirtiat _:; - 3M Environmental Laboratory Page 127 of 276 ReportE02-0443 .. Tenn River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0097.D Report Date: 27-Aug-2002 10:06 Page 1 3M Environmental Laboratory Data file E02-0443, Tenn. River Valley Samples : \\Etstargetktargetkchem\dudejr.i\D020629.b\DUDE0097.D Lab Smp Id: SL-2. C-I-3 Inj Date : 01-JUL-2002 05:53 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Misc Info : Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstargetktarget\chem\dudejr.ikD020629.b\D020629.m Meth Date : 27-Aug-2002 Cal Date : 30-JUN-2002 Als bottle: 54 09:59 dudejr.i 22:46 Quant Type: ESTD Cal File: DUDE0058.D Dil Factor: 1.00000 Integrator: Falcon ; Target Version: 4.12 Compound Sublist: all.sub Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compounds =.nmmmsmm..u.mmmm=wm===a=m 18 PYBS (299) : 20 pPHS (299) ; I '_ 21 pFOA (4139 ; 22 POSA (498) "{t 22 pPO_3 (4_) QUANT SiS MA88 m=mm 299 299 299 399 399 399 399 413 498 4_ 499 RT m_3.39'/ 3.169 3.750 2.795 3.394 3,S58 3.982 3,999 4.7(;2 4.I00 4.611 IXP RT _m.._=_. 3.381 3.381 3.381 2.792 3 .'/92 3.'/92 3.792 3.990 4,75G 4.161 4.1G8 DLT RT _m_=.nm= 0.00& -0.212 0.369 0.006 -0.398 -0.234 0.190 0.001; 0,001; 0.012 0.443 R68PONSB =mmmi._m 1134g 2189 1134 3a992 1197 8611 1879 12700 149S4 126853 11361 CONCBNTRATZON8 OH-COL_N PIN/EL (ng/mL) m=m === 1221._,2 1224.44 1224.50 0.03'/00 (ng/mL) o=mmm=_ 1220 1220 1220 0.0370 '/97.188 0.17(L9 797,169 919,045 0.02301 1274.02 1277.43 797 0.11"/ 797 819(M) 0.0230(M) 1270 1280 QC Flag Legend M - Compound response manually integrated. 3M EnvironmentalLaboratory Page 128 of 276 Report E02-0443 . .. Tenn. River Valley Samples Data File: \_tstaP[et%tar[et%chem%d_dejr.i%DO20629.b%DUDEOO97.D _,%EL_sarl:et%Lae'geL',_he_%dudre. i %DO20G29b.%DUDEO09I)7. 5.4" 5.2i Pal;e 2 4o8_ 4._4.44.2_ 4.03.8" 3.G" 3.4" 3.2:. 3.0" 2.8- >- 2.4_ 2.2" ,4 2.0:. 1.8- t.6" 1.4" a t.o- 0.8" 0.6-." 0.4-" u'2"ll IIII 0.5 1.0 t.5 iS PF'BS (299) II IIIL t-el II I 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 Hin Ion 299o00 3.32 : 3.0" I 2.7" _ 2.t; 1 1,5" 1.2: 'i _ =.8"_ i - i _ o i 3.00 3.2_|Z1,3.40 3.GO 3.80 20 PFHS(399) - ._ ,._oi /v_ II " _ _ i.zo" AI/ YI|1_ O.C)O.: 0.80i 0 , = , o - t = 3.40 3.60 3.80 4.00 4.Z0 Hin i-_,,_c.,...,.:-.. 3M Environmental Laboratory Paoe 129 of 276  Report E02-0443 _at, a File: %\Etstarli:et\barget._chem_,dudejr.i_)O2062).b_DUl)EOO97.]D 21 PFO_ (4t3) Ion 413.00 3.9; z.+: 3.0- 2.7-: v +':+\ 2.( 24" I_ "; l_ /I _..5" t2_ , . . , , , i 3.60 3.80 4.00 4.20 4.40 Htn 2Z FOSA <49e) Ion 4984 O0 9.0" (_ 'i o+o-:" t 7.0_ _ 4.o- 2.o i+o" :-.,., 4.40 23 PFOS (499) '; I_ 4.60 4.80 Hln IJ 5.00 6.20 2+2" 2.0" j ,.e4 ; 1.2-." 1 .o-.: _ o.a_ 2.4.: '= 0.2; I -./ - i - | -..-.....i 3+80 4.00 4.20 4.40 H|n 4+6<) ,.., .t . _ Tenn. River Valley Samples P;q[e 3 ExacCt opyof Original 3M Environmental Laboratory Page 130 of 276 Report E02-0443 . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0105.D Report Date: 27-Aug-2002 10:06 Page 1 3M Environmental Laboratory Data file E02-0443, Tenn. River Valley Samples : \\Etstargetktargetkchem\dudejr.ikD020629.bkDUDE0105.D Lab Smp Id: SL-2. C-3-2 Inj Date : 01-JUL-2002 07:21 Operator : mla Inst ID: dudejr.i Smp Info Mist Info Comment : Tenn. : : River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Method : \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m Meth Date : 27-Aug-2002 Cal Date : 30-JUN-2002 AIs bottle: 60 09:59 dudejr.i 22:46 Quant Type: ESTD Cal File: DUDE0058.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compoun4_ 18 pBS (299) 30 ppllS (399) 21 pPOA (4133 : 22 POSA (498) 33 p3po8 (499) ! QUANT SZG NA_S 299 299 299 ]99 399 399 4_3 498 498 499 499 499 RT l_(P RT DLT RT RBSPONSH CONCXNTRATIONS ON-COL_N FINAL (ng/mL) (ng/m_) 3.38I 3.162 3.7S0 3.790 3.$45 3.976 3.39S 4.769 4.427 4.174 4.434 4.005 3.381 3.381 3.381 3.792 ].792 3.792 3.9)0 4.756 4.756 4.188 4.1G8 4.158 0.007 -0.219 0,36S 0.006 -0.24? 0.184 0.80S 0.013 -0.339 0.008 0.266 0,437 9230 169G 2638 3298 490] 3370 8771 20521 144G 178402 85700 19535 1224.04 1224.47 1224,41 0.02S79 0.0714] 0.03784 819.284 0.25210 2744.26 o.,8883 1375.24 1377.19 1220 1220 1220 0.02S8 0.0T14 0.0278 819(N) 0.2S2 3740 o.917 1280 1280 QC Flag Legend M - Compound response manually integrated. _ ExacCt opy_,__r_"n- 3M Environmental Laboratory Page 131 of 276 ReportE02-0443 . _ Tenn RiverValley Samples Oata File: %%Etst,_rl;et,\t_t'l;et%che_\ducle_r.t%OO2GZg.bNOUgEOS.D N_JEt,star i;etNt, arl;e t%chemXdudej P. L_D020629. b_gU])E0105. D Pece 2 t.0- o.9- o.e" 0.7" 0.6" 0.5-" >0.4- 0.3" 0.2" 0.1-' ", _IJ..J,-J .... I.| , .... . * .... 0.5 _..O .5 m.... 2.0 J .... 2.5 Imf .... I 3.0 | * I.1..|. 3.5 I-*| _..L..| 4.0 * .... 4.5 Hin m .... 5.0 i .... 5.5 t_i_.... 6.0 i .... 6.5 = ....... i .... 7.0 7.5 * .... S.O i .... 8.5 * .... 9.0 t8 PFBS L:_9) ]on 299.00 I .. 3,0-.." I_ o ! It A/ ;: _ 2.2_ ._ _ 2.o-: _ II / _! _.,6- , / 1.2J m. i * , , , , 3.00 3.2_|n3.40 3.60 3.80 ZO PFHS 399) ! { Ion 399.00o iI ,.,o! ; _-_. ,, I,, =._o: I _ JI 1'_ I':'-_ l \J I fl I"_'*" I -[ _ I I. I'-*.";/N._ I Nit I '' _ / A, .I-'.._........... _ ,'7 I _.,o_.%o_._,_ ,.20 _aCt Cl;,; .... . _ _,* _ /-_Z_/__,/6"z- " 3M EnvironmentalLaboratory P_q_ 132 _f 77_ Report E02-0443 , _ Tenn River Valley Samples Data File: %_Etstarget_,tarcet_,che_,dudejr.i\DO20629.b_3)U_EOiO5.D 21 PFO_ (413) 3.4_ 32! z.oz.e- II Ion 413(I.-00or_. H (I 2.4 2.2-" 2.,\ I/ _Z.o" " 1.6_ 1.2! i - i o .i ..i o 3o60 3.80 4.00 4.20 4.40 H_,n 22 FO,%q (498) Ion 498.00 "I 1.2- :L.O- ^ 0.8-" >" 0.4" ** , . o . - , , 4.40 4.GO 4.80 5.00 5.20 Hiq 23 PFOS (499) 4.o" Ion 499.00 ' = 3z.8.2" _ _ i 22..04"" i _" 1o2:. 0.8" 0.4_ , Mtn _/_ I Pace 3 E_acCt_ I'i_I t:." 31 L_ :}ii.. 3M Environmental Laboratory Page 133 of 276 Report E02-0443 Tenn. RiverValley Samples , II Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0117.D Report Date: 27-Aug-2002 i0:07 Page 1 3M Environmental Laboratory Data file E02-0443, Ten n . River Valley Samples : \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0117.D Lab Smp Id: SL-2. C-6-I Inj Date : 01-JUL-2002 09:33 Operator Smp Info Misc Info : mla : Tenn. : River Valley Fish. Inst ID: dudejr.i Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Comment : Method : \\Etstarget\targetkchemkdudejr.ikDO20629.b\DO20629.m Meth Date Cal Date : 27-Aug-2002 : 30-JUN-2002 09:59 dudejr.i 22:46 Quant Type: ESTD Cal File: DUDE0058.D Als bottle: Dil Factor: 69 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compounds =u m_===mm_m=_=Rmn=R==_l==a 10 PPBS (299) 20 pPHS (309) 21 PPOA (413) 22 FOSA (496) 23 PYOS (69'J) _._ qt 'i , QC Flag Legend OOANT SIG MASS =u =,= 299 295 299 399 413 498 699 499 RT =s=w 1.380 3._76 3.750 3.798 3.996 4.7G9 4.1S1 4.605 EXp RT =,l ].3al 3.3$& 3.381 3.792 3.990 4.751; 4.266 4.168 DLT RT 0.007 -O.2OS 0.369 0.006 O.00G 0.013 0.023 0,437 RRSPON_E CONCENTRATIONS ON -COLt_N FINAL (ng/mL) (ng/m_) 9473 Iq10 1224.02 1224.40 545 1224.53 2433 0.00120 If00 a2417 221262 610.302 0.33013 2.2603S 22665 2277.10 1220 1220 1220 O.O0120(M) 61_(M) 0.330 3.2,S 1280 M - Compound response manually integrated. 3M EnvironmentaLl aboratory Page 134 of 276 Report E02-D443 | I I IIIII -_ Tenn. RiverValley Samples Data Fi|e: X_Etst.rcetXt.arEeb%che*,0_udeJr',i\DO20629.bXDU_EOlT._ 1.9" 1.8-_ 1.7" 1.6" XXEt staP_etXtaPet%ohe_\dudej r. i%D020629. bX_JDEOti7.D 1.4- 1.2" i.i_ i.O-." i: t 0.9" >" O.S" ; o.7-:. ; O,6" ; 5- i 00,.43- " Pace 2 ,i .... s ........ D .... I .... t .... 0,5 i.O i,5 2.0 2,5 3.0 3,6 4.0 4,5 5,0 5.5 6,0 6.5 7,0 7.5 8,0 8.5 9.0 Hin i8 PF_ (299) 3.2- 3.o- 2.8_ 2,6-." Z,4" Z.0_ Ion 299.00 ,.; > i.4= ", / *'LJ t.0 * , -, *-*,* 3.00 3.20 3,40 H_n 20 PFH$ (399) * * , * i 3.60 3.80 , 1_-" :.zo: I -_ : 7-'_" G._- _ Ion 3SS,O0 ! 0.70 i 340 3,60 3.80 4.00 4,20 Hln ExacCt opyofOriginal 3M Environmental Laboratory Page 135 of 276 Report E02-0443 .. Tenn. River Valley Samples Data File: %_Ets_arget_tar_et_,che_,dudeje.|\I)O20629.b%OUOEOl17.D 21 PFOI(413) Ion 413.00r," 2"4i Jl 2.z" I_ 2.0- j[ 3.60 3.80 4,00 4.ZO 4.40 H|n 22 FOSR(49e) Ion 498.00 0.9: 0.8-.: 0.7" v 0.4_ / _- 0.3" 0.2-: _ [ .: _.. = ,- J _ J - . i I.... 4.40 4.60 4.80 B.O0 6.20 H_n 23 PFOS(499) Ion 499,00.,4 4.o_ ,_ 3.6: ' I 3.2" 2,8" 2.0_ i 2.4- 0,8" _- t0.,24-" i *. i o i i 3.80 4.00 4.20 4.40 4.60 x|_ P_e 3 3M Environmental Laboratory Page 136 of 276 Repo_ E02-0443 II |II . _ Tenn.River Valley Samples Data File: DUDE0066.D Report Date: 27-Aug-2002 11:05 Page 1 3M Environmental Laboratory Data Lab Inj file : Smp Id: Date : E02-0443, Tenn. River Valley Samples \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE0066.D SL-3. C-2-2 03-JUL-2002 02:49 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 , Misc Info : : Comment : Method : \\Etstarget\target\chemkdudejr.ikD020702(D20702).b\D020702.m Meth Date : 27-Aug-2002 II:01 dudejr.i Quant Type: ESTD Cal Date : 03-JUL-2002 01:21 Cal File: DUDE0058.D AIs bottle: 55 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Concentration Cpnd Variable Formula: Amt * DF * CpndVariable Local Compound Variable Compounds QUANT SIG MASS RT EXp RT DLT RT RBSPONSE CONCENTRATIONS ON-COLUMN PIMAL (ng/mL) (ng/mL) 18 PFBS (299) 20 PPHS (:399) ; 22 PPOA (413) J 23 POBA (498) i 23 pFO8 (499) .,t 299 299 2_J9 399 413 4S8 499 499 3.395 3.103 3.757 3.819 4.003 4.803 4.181 4. f)91 3.387 3.387 3,387 3.791 3.989 4.748 4.167 4.16"7 0.00B -0.204 0.3"70 0.028 0.014 0.0S5 0.014 0.424 14872 3040 3238 S059 22949 23838 193614 239S4 1220.00 1230.48 1220.51 0.20394 0.27074 0.43100 1.14537 1324.22 1220 1220 1220 0.204(M) 0.2"21(M) 0.431 1.14 1320 4 I QC Flag Legend M - Compound response manually integrated. 3M EnvironmentalLaboratory Page 137 of 276 Report E02-0443 . _ Tenn. River Valley Samples !1 ' :_; Data File: _,%Etstarcet\Larcet\cd_m\dudejr.i_DO20702(D20702).b\DUUEOO66.D 2.9! 2,8_ 2.7_ Z.5" 2.4_ 2.3 i 2.2_ 2.1 i 2.o_ .94 1.8_ .7 i 1.6-." _..6i _.3> 1.2;: t.1 i 1,0_ O.8-.: 0.7 i 0,6-; 0.5" %%Et.stat'Ket;\barcet\_hem_dudePj. i\D020702( 1)20702) .b\DUDEO066D. Pace 2 0.2_ oo'1_ o.3i-..I..I J, I.I.I.r. l D.... 0.5 1.0 i .... 1.5 i .... 2.0 i, .... 2.5 Ii..-I. 3.0 18 PF_S (299) ;on 299.00 _. oe ....i.f... #l/'_.lll_=l.... e ........ 3.5 4.0 4.5 K.O 5.5 Hln I , .... , .... i .... J .... f .... a .... i .... 6.0 6.5 7.0 7.5 8.0 8.5 9.0 4.5" :::i 3.6" Jl r_ II >" 2.1" t.8" _.2"Le"_ 3._ 3._._ 2O PFHS(3_)) _.,_ _._ 2.4- z.o_ _ II _..4: ExacCto,poy f Origina_ _.o_. ,.,., 3.40 3.60 3.80 Hip , _f,,_--" 4.00 4.20 3M Environmental Laboratory Pa_e 138 nf 27_ Report E02-0443 ._ Tenn River Valley Samples Data File: %%Et.st.artet,',,kar.l_et.',_hQm_udeJr-i%lX>20702(_20702) 2_. PF04:I (413) 5.1_ 4.04.5_ 3.9- Zon 413.00 o T 3.0_ 22,4.-7-: 2,_.-: 1.8" 4t..52":_ . i I .i ...T . i 3.60 3.80 4.00 4.20 4.40 H|n 22 FOSA (498) 2.22,0 -." 1,8 i _,._- Ion 49a. oo _. to..eo_-." 0.6_ +.4-." 0.2_. ._-. ....* 4,40 j T I+ i - . I ' I * I 460 4.80 5.00 5.20 Hin 23 PFOS(499) Ion 499.00 3.3i ,4 3,0- _" "] 2.7" i 2+4" '_ 2,ti 0.9" 0.6" 0.3" I _ .i o o- 4.i o....o. ;o.z$4".4"0 i 4.60 , Htn .b_gE_6.g it Pabce 3 ExactCopyofOriQinaP 3M Environmental Laboratory Paae 139 of 276 Report E02-0443 Tenn. RiverValley Samples Data File: DUDE0076.D Report Date: 27-Aug-2002 i1:06 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE0076.D Lab Smp Id: SL-3. C-4-2 Inj Date : 03-JUL-2002 04:39 Operator : mla Inst ID: dudejr.i Smp Info Misc Info Comment : Tenn. : : River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Method : \\Etstarget\targetichem\dudejr.i\D020702(D20702).b\D020702.m Meth Date : 27-Aug-2002 Ii:01 dudejr.i Quant Type: ESTD Cal Date : 03-JUL-2002 01:21 Cal File: DUDE0058.D Als bottle: 62 Dil Factor_ 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Cpnd Variable Formula: Amt * DF Local * CpndVariable Compound Variable Compounds mRmsmumllmmmnmmmn_mm I wmmm. 18 PFB8 (288) 20 PWHS (299) ; : 22 TOSA (498) 3213 _Pl_O8 {(44,1939)) .; ! + QC Flag Legend M - Compound response QVANT BIG MASS mmmm 299 299 299 399 399 399 498 44193S 49ii 499 RT ms_m ].394 3.182 3.770 3.625 3.872 4,.010 EXp RT DLT lIT RESPONSg mmmmmmm_mmmnmmim n_mmmmm. "1.187 3.387 0.007 -0.20S 21275 2087 3.387 0.383 1284 3.7Sl 3.791 Q.034 -0.219 39G5 3286 3.791 0.219 3291 CONCRNTRATION_ ON-COLUMN PINAL (ng/mL) _mmmmmm 1219.74 1220.52 1220.55 O.1E277 0.16964 0.]E973 (ng/mL) mmmwmm_ 1220 1220 1220 0.14_ 0.170 0.170 4.769 44..011807 3.811 4.591 4.748 34...2_6[7'99 4 . _427 4.167 0.021 00..002;1_0L -O.3S6 0.424 20987 30?9914370 1247 20381 0.3;235 73).550.361(0;7 1324.61 1324.29 0.3;2 3.7$_1'S|M) 13_O 2320 manually integrated. .I + F-+xCacet_yofOriginal c+_,-,.._+._. ,, .... 3M EnvironmentaLl aboratory Page 140 of 276 Report E02-0443 . _ Tenn. River Valley Samples Daf.a File: %%Etst_set%t_l_et%chem_k_lejr.i_DO20702(D20702).b_DUOEOO76.D _Et_t_Ket\tarcet%che_dudeJr, 1.1- 1.0-" 0.9" 0,0O,7- "4-- i_D020702 ( D20702).b\nU]_O076. D i.'i 05- PaEe 2 3_ :i 0.2" .... i .... 0.5 18 PFBS(299) ) .... 1.0 ) .... 1.5 ) .... 2.0 | .... 2.5 t .... 3.0 i .... 36 a .... 4.0 ) .... 4.5 Hin i .... 5.0 i .... 5.5 o .... 6,0 ) .... 6,5 ) .... 7.0 i .... 7.5 ) .... 8.0 i .... 8.5 i .... 9.0 i Ion 2_9,00 4.z:. |- , 3.9,: / / , 3.3" / 2.7" / .!i v_ 2.4" _/ ; T ./ : ='=: _,,/ 7 I. z-.'.__...._._ 3,00 3,20 3,40 3.60 3.80 Hin 20 PFHS (3_) i Ton 399.00 ' _.5_ _ J_ ,; ExacCt opoy:Or;_linaJ 0.8- 3_40 3._0 3.80 4,00 4.ZO H_n 3M Environmental Laboratory c_,_,= _ _ 9v_ Report E02-0443 . _ Tenn. RiverValley Samples Data File_ \%EtstarEtt%tarEet%c_Xdude_r+i_OZO7O2_O7OZ) 21 PFOA (413) Ion 413.00 3.2- _o :::i/ fl i Z.o- > 1.6" i04_ . . i , o i...i 3.60 3,80 - 4.00 -1 -4.20 .i 4.40 22 FO_ 7.0_ (49_) Ion 498.00 : 6.0:. ; S.O-_ :1 i 43.0.o_ -_: ,.fi\ + i - i . i i " + 4.40 4.60 4.1B0 5.00 5.20 23 PFOS (4_) ; Ion 499.00 . 4.4" 4.0-_ 3.2-" 2.8-" 2.4" ii1 i 32.6.o4 _ i.2i o.o_ _; j 0.4 _. :I i It / i i i 3._ 4,00 4.20 HJn _, I i 4.40 4.60 ._%_U_0_760_ Pa_e 3 O 3M EnvironmentalLaboratory p=,o _9 _+9v_ ReportE02-0443 - _ Tenn.River Valley Samples Data File: DUDE0083.D Report Date: 27-Aug-2002 ll:06 Page 1 3M Environmental Laboratory Data file : Lab Smp Id: Inj Date : Operator : Smp Info : Misc Info : Comment : E02-0443, Tenn. River Valley Samples \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE0083.D SL-3. C-6-1 03-JUL-2002 05:56 mla Inst ID: dudejr.i Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun Method Meth Date : \\Etstargetktargetkchemkdudejr.i\D020702 : 27-Aug-2002 ll:01 dudejr.l Quant (D20702) Type: ESTD Cal Date : 03-JUL-2002 01:21 Cal File: DUDE0058.D Als bottle: 68 Dil Factor: 1.00000 .b\D020702 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 02 .m Concentration Formula: Amt * DF * CpndVariable I Cpnd Variable Local Compound Variable C(_pounda =:==ms_m=m===== == mmnw_n=_ 111 pFBS (299) r 20 pPItS (3S9) ; 21 PFOA (413) , 22 FOSA (498) _3 pFO8 (499) QUINT SIG MA.%_ s=m= 2%9 3'JS 413 4%0 499 RT EXP RT DLT RT m=== _mwm_ ns m lu_=sm RESPONSg ==nmmu== Compound Not: DetectRd. co_,poun4L blot. De'ceted. Coipound Compound Not Detecned. Not Detected. Co_pound Not Detect:e,*1. CONCENTRATIONS ON- COL_aN YZMAL (ng/mL) =_==.== (ng/mL) ===_l_= "i 3M Environmental Laboratory !-::_cCt opoyfOdg|naJ :,C+ ,li Page 143 of 276 Report E02-0443 . _ Tenn River Valtey Samples 3M Environmental Laboratory p=,,o 4,_,__ '_-rr i Report E02-0443 --- Tenn. River Valley Samples Data File: _._Ebstar'get,\taret.'_chem\dudejr.L',,_O20702(D_702).b_OO83.D 24- P_OA<4t3) (Undete_c_d) 408-. TOn4t3o 4G5_ 403_ >"4oz_ 40"1- 2 4 6 8 10 22 FOS_ 4498) (Undetected) 20G-: ton 498.00 206_ _ 2o4- 2o3- 2o2_ ::_ :L99_ lc)8_ _L97_ 2 4 6 8 1o H_n : 23 PF'OS(4_9) (Urtcieet,mf,@d) Ion 4"_ OO 3_.5.: at,_ zto" _, _" 3o9" I _oe=. 2 4 & 8 _.0 i Pace 3 _,:",;C;. opyof Origin_ '_i_al Oat_ 3M Environmental Laboratory Page 145 of 276 Report E02-0443 il 11IIIIIIII Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0065.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.bkDUDE0065.D Lab Smp Id: Water Blank-I Inj Date : 12-AUG-2002 23:11 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443 Water Blank Water Samples; non-GLP; 6/20/02; OK Misc Info Comment : Method : \\Etstarget\target\chem\dudejr. Meth Date : 27-Aug-2002 14:06 dudejr.i Cal Date : 12-AUG-2002 16:13 AIs bottle: 20 Dil Factor: 1.00000 i\D020812A.b\D020812A.m Quant Type: ESTD Cal File: DUDE0027.D Integrator: Falcon i Target Version: 4.12 Compound Sublist : all. sub I I Compotmdm Illlnllllillml I Illl I nllnll I P1_138 (299) 2 P_:_ (399) :3 pih0A (41.3) 4 POSA (498) :; 5 9FG.S (499) 0UAMT SZG IIASS II I I 299 299 299 ;999 299 411 495 495 _ SXP RT IIii I I IIIIII 3.353 3.209 4.201 _J.00t _1.51;5 4,010 4.809 4.301 3.394 3.394 3.394 3.?)1 ].791 3,9112 4..258 4..Lt;O o'r.T _ ii I lllll -0.041 -0.155 0.807 0,013 -0.321; 0,034 0.041 0.041 R_PO]_qll l Ill Iiii 29174 $546 1504 5192 1012 9L79 3390 34010 _N_K%YZ_ATI O_ ON-COLUMN (ng/mr_) l I llll_ 0.54141 503.(;60 503,788 0.15468 0.0270] 0.04921 0.10549 0.16998 P][NA_ (nglmL) IIIIIII 0.541 S04 S04 0.155 0.0270 0.0492 0.1.05 0.1"20 i : 3M EnvironmentalLaboratory E;cac_Ccu7 c:; ' .' MI_.aJ Date Page 146 of 276 Repod E02-0443 . _ Tenn. R_er Valley Samples Data File= \_Etstar_e_%tar;e_che_dudejr.i_O20812A.b_J_EOO65.D 2.1_ 2.O_ i.9' 2.917, i.6" 1.5" 1.4! 1.3-_ 1.Z" _Etstar _et%_.ar _et\ci_m\dude_ r. i _DO20812A. b_)U_EO065. D ii..Oi- " O.e" 0.7 0.6" Pa(e 2 "ij jj, 0.3.",i 0.2 _ ........0..5 i.0 " ....._....5.......2....0.........2...5........3....0 3.5 4.0 4.5 5.0 i'g .....6....0.... 6.5 7;i .....7...5........8...0.... 8.5 9.0 Htn 1 PF3S (2_9) 4.e" 4.4" ! ,.o-: ! 36-; ' 2.8- , :- Z.O-: _; I, qJ 2.4 2.8 2 PFHS(3c_) ........... 3.2 3.6 4.0 MAn _)0: Ion 3'_ O0 ':_ ExacCt e,_,y-._,:::;,-;::.:.-: doo_ _.,o_._._o ,._ ,._ @ 3M Environmental Laboratory Page 147 of 276 Report E02-0443 Tenn. River Valley Samples "- Dal_ File; %_Etst_el;et\f_get_cl_m%dudeJr'i_d_O2OEL1_R'b_])UDEO0$5"_ 3 pFOR(413) Ion 4t3.00 r,- 2.o_ 1.6" "" t.4-: I_ "_ I fl 1 t.0" 0.8" * J\ / 0.6_ o.._| 3._ 3.,_,,.oo4.2o,.,o] 4 FOSR(498) eSO._ ]o_ 498,,00 o = '; 700" SO-.' 5oo- 4_-:. , i ! i . ..i,." 4.40 i.,,i ." "| ...i 4.60 4.90 S,.O0 I_,._0 Hln i B pFOS (499) 15.B_. S+O-',: 4.5" Ion 499.00 i ZoO" to5-_ ) o.5"_ .. ....... 3.BO 4.00 4.20 4..40 4.GO .I i Pace 3 Exa_Copy_',_=c:;i Inili_ " 3M Environmental Laboratory Page 148 of 276 Report E02-0443 Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0066.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory Data Lab Inj file : Smp Id: Date : E02-0443, Tenn. River Valley Samples \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0066.D Water Blank-2 12-AUG-2002 23:22 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443 Water Blank Water Samples; non-GLP; 7/17/02; OK Misc Info Comment : Method : \\Etstarget\targetkchem\dudejr.i\D020812A.b\D020812A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Date : 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle: 21 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Compo_mdm mmmmmmmmmmmmimmmlmmmmlm_mm 1 pFBS (299) 2 PPHS (399) 3 pPOA (413) 4 POSA (495) 5 PPOS (499) Q_ 8ZG MA88 m.Mm 259 299 2S9 299 399 423 413 498 499 RT RXP RT mmmm m_mmlm_m 2.354 3.394 3.210 3.394 3.743 4.195 3.354 ].B94 3.805 3.791 4.010 4.359 3.982 3.902 4.110 4.201 4.758 4.160 DLT RT _PONBI mmmwmmmm mmmmmmmm -0.040 54510 -0.184 10519 0.349 0.801 1278 3550 0.014 4219 0.02s 0.277 1174_ 1059 0.042 0.041 3372 33507 CONC_'I'KATXON8 ON- COLI,_N PINAL (ng/mL) mmmm.m, 1.4337_ 503.482 503.011 503.727 0.12496 0.21475 401.976 0.10487 0.15720 (ng/_) mmm_mnm 1.43 503 504 504 0.125 0.215 402 0.105 0.157 3M EnvironmentalLaboratory Page 149 of 276 ReportE02-0443 m Tenn. RiverValley Samptes Dat.t File: %%Etsta,'_et%tar,et%chtm%dudejr.iX_G2G812_i.bX])U]DE@G66.D %_tstarget%t artet%ol_m_udejr. L'_)0208t2R. b"_U_KO066. D PaEe 2 t8 i 'l7! _..6-_ d.5" _.3" t.2- ::L.O-: 1_.4_: 1 :,- 0.9 i O.B" 0.7: 0.5" 0.4: 0.3" o.2 O'6I'" o.5 _L.O .5 2.0 2.5 3.0 3.5 40 4.5 6.0 6.5 G.O 6.5 7.0 7.5 8,0 8.5 9,0 H_,n 1 PF)S(299) , Ion 2J9O_ 14 r; ', 0.9" ! 08" ' 07" ?._ O.G" t O.5" O"1!= e = 2.4 2.8 3.2 | = 3.6 4.0 2 _ (399) : eeo_ xon _.oo I e4o_ I 7so" ". eao,- 4oo- , 3.40 3.60 3.80 4.00 4.20 Bin ,J_3CtC_, _.::i);:._ , _ -lJ_al Data 3M Environmental Laboratory Page 150 of 276 Report E02-0443 Data File: %_EtstarKet%tar_t_.ht_udeje.i%lDO20S_2R.b_J_U]DEOOG6.D 3 PFOA(4_.3) [on 413.00 z.44 2.2: 2.0E i.S-_ i _> t. 6-.: " 1.2" _" 1.0" o.g-:. 0.6-: _ . / 0.4".,-_. ,_ _ . ..... 3.6Q 3.80 4.00 4.20 4.40 Hi_n 4 FOSA (4_) _o- 64O-." Ion 498.00 o _ 32O . . _ . o . i . . o . D. , , t 4.40 4.60 4.80 5.00 5.20 H|n 5 PFOS(499) , 5,,53 Ion 49_00 N ; 5oO_ ; 4.8_ I ! 40-_ '. 3.s" ii! i "" i.S-_ t.0-_ 0. _-': j ./ 3.80 4.00 4.20 4.40 4.GO H|n :i . _ Tenn. River Valley Samples Pa(e 3 r,ractCo,o;..O.,.::..:: 3M Environmental Laboratory Page 151 of 276 ReportE02-0443 . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020{12A.b\DUDE0076.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.ikD020812A.b\DUDE0076.D Lab Smp Id: 38032 Inj Date : 13-AUG-2002 01:12 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443-38032; Water Samples; non-GLP; 6/20/02; OK i Mist Info : Comment : Method : \\Etstarget\target\chem\dudejr.ikD020812A.b\D020812A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Date : 12-AUG-2002 Als bottle: 26 16:13 Cal File: DUDE0027.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub compouncbl mi._smilmiBmm.nt_Bmml_m_mmn I. PPBB (299) 3 PPH _1 (299) 3 PFOA (413) 4 P08A (490) i S PPOS (499) i ;i I } 9ZG MASS aiJnae 299 259 299 299 299 399 339 413 490 499 RT limm 3.401 2.540 3.203 3.810 4.044 4.215 3.00S 4.003 4.789 4.181 RXp RT 81mwmmim 3.'194 3.394 3.394 -1.394 3.394 3.394 3.791 3.882 4.768 s,.11;0 DLT RT ml_mm.s, 0.007 -0.854 -0.191 0.424 0.650 0.821 0.014 0.021 0.031 O.02f RESPONSE unln_l.m 19"161 147211 1966 2962 758 777 15729S 84190 130473 190157 COI'41U_'I'P_T_ ONS ON- COL_N FZNAL (ng/mL) _.lmmmt 0.19664 4.72622 503.786 J;03.?51 503.028 503.037 4.85808 4.94452 4.S6920 5.10901 (ng/mL) ._lna.s 0.197 4.73 504 504 504 504 4.86 4.94 4.S? 5.19 3M EnvironmentalLaboratory Page 152 of276 Report E02-0443 I I . _ Tenn River Valley Samples +_ ])aba File: %_Etstarge_%target_r_eM_dudeJr.i_)O20e_2_.b_)UDEOO76.D 2.5: 2.4-:. 2.3" 2.2" 2._" 2.0_ 1.9: 1.8" '1.7 _. %_Ets_EetN_;e_%_m_ke j r. i%_02OB12Ab,_DU_EO076. Page 2 i _.. >" t. 0 -:,' 0.9: o.a" , 0.7" ; o.6_: 0.5=" t; _ i 0.2_ .... o .... i .... o .... t .... | .... t....i 0.5 1.0 1.5 2.0 Z._ 3.0 I PFBS <299) Ion 299.00 .... 3.5 e .... 4.0 i .... i .... 4H.1l5n _.0 i .... 5.15 i .... 6.0 t .... 6.5 p .... 7.0 i .... 7.5 o .... a.o = .... 8.5 i .... 9.0 3.6" 3.2-_. _,_ tt4 O o.4_ : 2.4 I 2.8 _ I,, ___,_ _ _, t_ 3.2 3.G 4+0 ;an 399.00 : 3.6- i ]._" I 3.o- I =.r I Z.4- i.e-: ). _l.. 2" 0.9" 0.6_ 03i _t 3.40 3.60 3.80 4.00 4.20 Hin . ExacCt opyofOriginaJ _nIU_ Date 3M Environmental Laboratory Page 153 of 276 Report E02-0443 Data File*. %\EtstarEet%tarl:et%-.3_m%dudejr,i%DO208J_-q,b_l)UDEOO76,D 3 PFOA (413) Ion 413. O0 v i 6-.: 1,4-_ 1.2" :,- 0.6:. 0.4" 2-.: * 3,60 t ' * .... __1 -- 3.80 4,00 4.20 4,40 M_n 4_ (496) Ion 498,00 2.2" _i 2.0" ' l. 8-." i 1.6! '!' 9 t.4" _i, 1.O! _ v o.a- :" 0.6" 0.4" 0._ , __ , " * D - | * " i - - * ! * 4.40 4,60 4,80 5.00 5.20 Mi_ PF'OS (499) " 3.6- Ion499,0=0 ,, 3.3" _ ; 3.o_ .! 2.7" = 2.4: I ^ 2.1-_ / _; > 1.z:. j : 0.9-'. 0.6_ 0.3" .. I * i *,*. I a- * | 3,80 4,00 4,20 4,40 4,60 , Hin . _ Tenn.River Valley Samples Pal;e 3 3M EnvironmentalLaboratory Paoe 154 of 276 ReportE02-0443 Tenn RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\DO208"12A.b\DUDEOO73.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0073.D Lab Smp Id: 38029 Inj Date : 13-AUG-2002 00:39 Operator : mla Inst ID: dudejr.i Su_p Info : 002-0443-38029; Misc Info : Water Samples; non-GLP; 6/20/02; OK Comment : Method : \\Etstarget\target\chem\dudejr.i\DO20812A.b\DO20812A.m Moth Date : 27-Aug-2002 Cal Date : 12-AUG-2002 Als bottle: 25 14:06 dudejr.i 16:13 Quant Type: ESTD Cal File: DUDE0027.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub _ laRlma.mlm=lm_m.m=_mmwm.mR 1 PPB_ (299) 2 PP_IS (399) 3 I_OA (423) 4 POaA (495) 5 pFO,_ (499) OUANT SZG MASS amn_ 299 399 413 498 499 499 RT _ R'_ m=mn _fs=g=l_ 3.400 3.511 3.394 3,791 4.009 3.902 4.796 4.187 4.768 4,180 4.467 4.260 DLT RT gmm.mw=m 0.014 0.020 0,027 0.028 0.037 0.307 RBS_S_ "n==B=ai 89092 252177 3280B_ 34000 631588 131570 CONU"_NT1KKTZO1k'lS ON- COLOMN FZNAL (ng/mL) m=m_.== (ng/wL) mmn_mRm 3.65591 7.55220 _.$G(M) 7.85 21.0621 21,8 1.21439 20.1841 1.11(M) 20.2 3.29049 3.29 QC Flag Legend ; M -_ Compound response manually integrated. ! '4 ; 3M EnvironmentalLaboratory Page 155 of 276 Report E02-0443 . _ Tenn. River Valley Samples 3M Environmental Laboratory Pane 15R _f27F; Report E02-0443 Data File: \_Etstaret\t_'et_che_%dudejr, i%l)O2082R.b_DUDEoo73.D 3 PFOR (413) ion 4t3.00 7.0- ; 6.o-: " 5.o_ x 3.0- >" 2.o- i _'0: !-- i i _._ ;._ _.'o__.'zo ;.'4_ Hln 4 FOSA (498) Zon 498.00 4.a_ ,; , 4,4_ ; 4.0- 3.6" r_ 3,2- i_ v 2.4-.." , _. 2.0" 1,2'" _" J oo o4:.......... : 4,40 4,60 4480 E.O0 5,20 Hin i 5 PFOS (4)9) i.o- ' ! Ion 499.00 ,4 o.9- : o.8" ', 0.7- i! i i, 0._" .-{ _ 0.4- " >" 0.3_ 0,2- 0.1_ 3,80 4,20 4.40 4,GO Tenn River Valley Samples mmlmmmmm Pae 3 ExacCt opyof Cd;;n-, [nif_ Dat_ 3M Environmental Laboratory Page 157 of 276 Report E02-0443 . _ Tenn.River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0130.D Report Date: 29-Aug-2002 07:12 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020al2B.b\DUDE0130.D Lab Smp Id: 38030 Inj Date : 13-AUG-2002 11:08 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443-38030; Misc Info : Water Samples; non-GLP; 7/17/02; OK Comment : Method : \\Etstarget\ Meth Date : 29-Aug-2002 Cal Date : 13-AUG-2002 Als bottle: 42 target\chemkdudej 07:08 dudejr.i 06:44 r. ikD020812B, bkD020812B, m Quant Type: ESTD Cal File: DUDE0106.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub [ i i i Compoumds mmnmmmmmmmmmmRmmmmmmllmmmmm 2 PI;'EIS (299) 2 PFHG (399) 3 PPOA (413) 4 08J& (498) 5 PFOS (499) QUANT SZG MASS mmllm 299 299 299 299 399 413 498 499 RT _111mm 2XP RT nmgmmmmm 3._a7 3.394 2.498 3.203 3.777 3.994 3.394 3.394 3.777 3.9(;0 4.741 4.139 3.791 3.902 4.7(;0 4.1(;0 DLT RT nmmnmmm, -0.007 -0. 891; -0.191 0.303 -0.014 -0.014 -0.027 -0.021 R_PONSB mmmm.ms= 197441 1231 2246 1_1260 0307299 4152125 7900357 8914428 CONCSWI'RATI ON3 ON- COL_4N plr NAL (ng/_) mm_=== (ng/mr.) = m==== 2926.50 2935. (;6 2935.62 2935.20 424.11;5 427.860 300.226 423.(;73 2930 2940 2940 2940 42_ 420 300 424 3M EnvironmentalLaboratory !_itla( u_t_. PaaP.15_ e_776 Report E02-0443 .. _ Tenn. River Valley Samples 3M Environmental Laboratory _.,_ , _ ^, ,-,_e Report E02-0443 Tenn. River Valley Samples _ta Fi|e: %\Et.starl;et.\tarl_et,\ohem%dxM:lejr.i\DO208_.b\_O130.D 3 PFOA (4t3) 7,0-" I ^ e,o:. !_ 4.04 "_ 3.0: ]on 4_.:300 _..0i " z.o:- 3.r_ !/ ! 3.80 4.00 4.20 4,40 M_r_ 4 FO$_ (498) ' Zon 498.00 , 0.9 i ' 0,8_ 0.6-.' !i' i 0.78-._'. )" 0.3i = 4.40 s 4,_, 4.80 Ht_ 5 PFOS (499) I 500 5.20 Ion 4_).O_ 2.2" :! &,O* i ,! _ 0.6- ! !. j 0.4" 0.2-: e 3.80 I -, * 4.00 i . * i .... I .,,* 4.20 4.40 4,0G tff,'_ i I Pal;e3 ExacCt o._,y. .... !nJt!a_ !::: 3M Environmental Laboratory Page 160 of 276 ReportE02-0443 Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0092.D Report Date: 27-Aug-2002 14:12 Page l 3M Environmental Laboratory Data file E02-0443, Tenn. River Valley Samples : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0092.D Lab Smp Id: 38043 Inj Date : 13-AUG-2002 04:09 Operator : mla Inst ID: dudejr.i Smp Info E02-0443-38043; Misc Info : Water Samples; non-GLP; 6/20/02; OK Comment : Method : \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date : 27-Aug-2002 Cal Date : 12-AUG-2002 AIs bottle: 34 14:06 dudejr.i 16:13 Quant Type: ESTD Cal File: DUDE0027.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Compounds mmmm=_=.m.mmmmmms==.mmmmm8 1 ppBrt (299) 3 P_I_J (399) 3 PPOA (413) 4 P0qA (498) 5 PFOS (499) :i I QUANT SIG MASS =mm= 299 299 299 399 299 399 413 498 499 RT BXp RT s==sm n_===m=. 2.3r-4 2.451 3.210 "t.394 3.394 3.394 3.018 4.037 3.962 4.010 4.796 3.394 3.394 3.791 3.982 4.?];9 4.195 4.1(0 DLT RT =m.B==== -0,040 -0.943 -0.I54 0.424 0.643 0.171 O.02B 0.028 0.035 RBSPONSB _.===.=. 32848 7:)9 6286 1244 1953 16543 .9481 I;471 30951 CONCENTRATIONS ON- COL_N FINAL (ng/mL) ====.=. (ng/_L) =.=_m=. 0.670(;1 503.839 503.634 0.671 S04 504 03.911 503.786 0.50173 0.0];858 0.201;98 ];04 504 0.];02 0.0];87 0.207 0.07297 0.0330 E'{acCt opyr,: O;."._ic,.., @ 3M Environmental Laboratory Page 161of 276 ReportE02-0443 IIII I III . _ Tenn. RiverValley Samples l)lta File: %%Etstirget_target_chemXdude_roi_,]lO20812Rob\])UDEOO92.D \XEt st a_get_t a_et %he_\dude j r +i %_020822A. bXDUgEO092. 2.0" 1.9" 1.8-: 1.6! i.e" 13! 1.2:. =i" l.O_ ; 0.8" 0.6J o._- Page 2 ......0..5......i..........i..5..... 2.0 2.5 i;; ....3...5......4..0.......4...5......5...0......5...5......6...0......6...5.......7..0. 7.5 8.0 8.5 9.0 Hiiq ,,. i PFBS (299) i xo,.z, _.% I 6.o_. g = 4.5" 4o0_ _ 3.t5" _._ =._ I :" Z.O'_ o _ _I _ _ ,! 0.5"_ 2.4 ...... 2.8 3.2 Hin ,... ,. . . 3.6 4.0 2 PFHS (399) Ion 3c_ +O0 .. .,.6- +i z.4- z.z" 2.0..: + ='"; /t"_, I_ I_ fl It. _..r .:,-.,. ;, OtiS[hal .( .L',S.L!Z. J.L_o _- :" l.O" 0.6" v _0..42-:"_ ........ ........ 3.40 3.60 3.80 4,00 4,20 H|n 3M EnvironmentalLaboraton/ p=_= 4no _=97= ReportE02-0443 ])ata File: %%Etstarget%ta_l[et\chem\dudejr.L%])O20812(_.b\_U])EO092.3 3 PFOA (413) 2.2: z.o: Ion 413.00 o _- o_ tl ,r 2.6" 11,.48"- ]/ __ i.o" o.e: 0.6- 4 FOSR (498) Ion 498.00 :1..4,,; i r- tt..i2i i 1 _.o" / v '"1 / 0.7_ / "__ .... .'m,_/,.. 4.40 4.60 4.80 5.00 5.20 H_n PFOS (499) 4.e_ Jl ; :t 4.o" : 44._ It 3.2" 2.8" 2.4: ="i._" :1.o2_ o.e_ 0.4-:_- tl/ ___ j _.'_ ",;.'_, ;o.'z',;;I._$" ;I.'6o H_n - - Tenn. RiverValley Samples Page 3 _,,.__,_!,. ,,'...: .... ..-_.C./_/ /_/,_,...  ReportE02-0443 - - Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0067.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0067 .D Lab Smp Id: 38025 Inj Date : 12-AUG-2002 23:33 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443-38025; Misc Info Water Samples; non-GLP; 6/20/02; OK Comment : Method : \\Etstargetktarget\ Meth Date : 27-Aug-2002 14:06 Cal Date : 12-AUG-2002 16:13 AIs bottle: 22 Dil Factor: 1.00000 chemkdudej dudejr.i r. ikD020812A.bkD020812A.m Quant Type: ESTD Cal File: DUDE0027.D Integrator : Falcon Target Version: 4.12 'l Compound Sublist : all. sub !_ Compound= mmzmmmmmnmmmmmmmmmmmmmmmmm 1 PFB8 (298) 2 PFHS 3 PFOA (3_)9) (413) 4 FOSA (49|) 5 pFOS (498) Qu,,ms.,zr g MASS nm mm 299 39) 413 498 499 499 CON_N%_KAT_ON8 os-col,_ FINAL P-T gXP1_ DLTK'T RI_SPONSli (rig/ran.I,,} (ng/mL) mmmm mmsNmmmm mmnmmmmm mmmmmmmm mmmmmmm mm_mmmm 3.401 3.394 0.007 91153m 2.99206 2.99(M) 3.822 4.003 3.';91 3.902 0.021 0.021 247750 321649 7.71134 21.3198 7.71 21.3 4.796 4.766 0.026 29388 0.96228 0.962(M) 4.181 4.260 0.021 503658 16.4924 18.5 4.460 4.160 0.30_ 135043 3.4025.4 3.40 i QC Flag Legend : M - Compound response manually integrated. t i 3M EnvironmentalLaboratory Page 164of 276 Report E02-0443 . _ Tenn. River Valley Samples ]Data File: \%Etstarl;et%tarcet_che_ludejr.i_DO20812R.b%_JDEOO67j) %_ t staPI;et %t_rget,%chem\dudej P. L%]DO20812R. b_DU_EO067. ]_ 2,O" 0.9-_ o.e; 0,7: Pal::e 2 o.s- >- 0.3" 0.2" .... * .... i .... i .... * .... g .... i .... | .... * .... i .... i .... i .... i .... i .... , ........ 0.5 t.0 1.5 2.0 2.5 :3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 Hln 1 PF]S (299) ;on 299.00 * .... p ........ 8.0 8.5 9.0 2.4" r_ 2.1" 1.S_ i 1.5: 1.2-" I1 .," i * * i * *i t* * i * * 2.4 2.8 3.2 3.6 4,0 Hin 2 PFHS (399) Ion 399.00 ' 4.o.:" a.s 2.5-," 1.5to0_ 3.O- /_ * s * . * D* I I - i 3.40 3.(_0 3.80 400 4.20 H_n [!t_C / ,-- . 2---- '' 3M Environmental Laboratory Paoe 165 of :?76 Report E02-0443 - - Tenn. River Valley Samples Oata File- %\Etstar_et_tar_et%ohe_JdejP.i%OO2OSl2R.b_I)U_EOOGTD 3 PFOA (413) Ion 413._ 6 0-." S.O" 43.0._o! >" 72.,0-_ I_ :-- I i e i, o, _..-o 3.60 3.80 4.00 4.20 Mln 4 FOSR(498) I 4.40 Ion 49B.00 4.0" " 3.6. _ z.o! 1.6-: 2.4: 0.8" 0.4: .".--.-'_,.'. 4.40 At /" , . . .", 4.60 4.80 M|n _.OO 5.20 5 PFOS(499) ioGO_ 0o90_ 0._" Ion 499.00 :I o.7,!= _ o.4o_ O 20 -'." O.tO_ 3.80 420 4.40 4.60 : PaTe 3 /:.:.... "=_ _(.:,,1"3., : -_.,... 3M Environmental Laboratory r_ , _., ,,-,_- ReportE02-0443 . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020B12A.b\DUDE0069.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory Data Lab Inj file : Smp Id: Date : E02-0443, Tenn. River Valley Samples \\Etstarsetktarget\chem\dudejr.i\D020812A.bkDUDE0069.D 38026 12-AUG-2002 23:55 Operator Smp Znfo Misc Info Comment : ntla : E02-0443-38026; : : Inst ID: dudejr.i Water Samples; non-GLP; 7/17/02; OK Method : \\Etstargetktargetkchem\dudejr.i\D020812A.biD020812A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Date : 12-AUG-2002 AIs bottle: 23 16:13 Cal File: DUDE0027.D Dil Factor: 1.00000 _ntegrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Compoun_ m''mmmm .mmi.1 .mmimm.im.m , I PPB5 (295) ! 2 P_I8 (395) 3 PPOA (413) 4 OBA (498) S PPOS (499) gVA/_ 8Za MASS 299 2)) 413 4)B 499 4gg RT 3.401 3.811 4.003 4.71g 4.160 4.4_ IXp RT 3.394 3.791 3.982 4.766 4.160 4._0 DLT RT RBSPONSB 0.007 0.020 0.021 0.021 0.020 0.3Q7 118S6? 255886 340061 31162 648655 14016 CONCBNTR.ATZON..q ON-COL_N pZNA/, (ng/mL) (ng/mL) 3.70420 7.95948 22.;$24 1.02079 20.7905 3.5S_1 3,70(N) 7.97 22.; _.02|N) 20.6 3.57 QC Flag Legend M - Compound response manually integrated. 3M EnvironmentatLaboratory Page 167 of276 Report E02-0443 . _ Tenn. River Valley Samples Data Ftle: %_tst_get\t_get%chem%dudeJr.i%_2_t2A.b%DUDEO_9.D 1.2- _st_rce_t _et_Xclude j r. i\_2081_, b_)U_G9. D Pace 2 0.9_ 0.72 i 0.62 > 0.5_ 0,3_ !0.4_ !I1t ! tt .... , .... i .... i .... , .... , .... . .... , .... ,o .............. 0.5 1.0 _.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 55 6.0 6.5 7.0 7.5 8.0 8,5 9.0 Htn PFBS (299) i 3.0, I_299_ ,; 1.8S II 2.4 2.8 3.2 3.6 4.0 Hin 2 PFHS (3_) _.0_ 5.o_5""_ . ! 40_ 23..50_q 2.0_ 1o0_ ". D , , . 340 3._ 3.80 4.00 4._ Hin _aCLCo_yo_Or_o_l_ 3M Environmental Laboratory p_r,= 1=_ ,_f _7_; Repod E02-0443 . _ Tenn. River Valley Samples ga'r,aF_lel \\Etstarget%tar=et_chqm%dude_r. t.\]BOZ08_-2A.b%DU_O069.D 3 PF(_ (13) Ion 413%00 7.0-" 6.0tS.O_ i 4.0" >" 2.0_ 1.0-: :_:-- , * 3,60 I - - m i 3,80 Hin 4.00 - J' 4,ZO I i 4,40 4 Fos,q ('498) lot1 498.00 4.84o4-: 4.0-_ 3.63.2 Z.4-; :_ 2.0_ I: 'i j 4,.40 4.60 4.80 _.00 5.Z0 I Mln 5 PF0S (4_) Ion 4=_.o0 _ :i 0.8_ 0.7" l.o_ ! .5" v OQ4_ " > 0.3_ ,; = 00.oZ1_". A Min 3,90 4.00 4.20 4.40 4.160 '_ Page 3 ["_,_',.I_ 3M Environmental Laboratory Paae 169 of 276 Report E02-0443 . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0071.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory Data file E02-0443, Tenn. RiverValley Samples : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0071.D Lab Smp Id: 38027 Inj Date : 13-AUG-2002 00:17 Operator : mla Inst ID: dudejr.i Smp Info Misc Info Comment : E02-0443-38027; : : Water Samples; non-GLP; 7/17/02; OK Method : \\Etstarget\target\chemkdudejr.ikD020812A.b\D020812A.m Meth Date : 27-Aug-2002 Cal Date : 12-AUG-2002 Als bottle: 24 14:06 dudejr.i 16:13 Quant Type: ESTD Cal File: DUDE0027.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Compounl= mmmmmmmnmmmmmmmm.mm_mmmnmm % PPBS (299) 2 PPH8 (399) 3 ppOA (413) 4 POSA (49|) 5 PFOS (499) QUA/_ S_G MA_S mmn. 299 399 413 49E 499 499 49_ RT mm=. 3.401 3.812 4.002 4.796 4.180 3.155 4.46? RXP RT DLT RT R_PONSR mmnmmmmm nmmmmmmm mmlmummm 3.394 3.791 0.007 0.020 102029 405593 3.902 0.020 412129 4.750 0.025 12_332 4.160 4.1G0 4.160 0.020 -0.%94 0.307 906339 4_01 85093 CONCBITL'RATZOL_ ON- COLTA_N FINAL (ng/mL) =mmmmnm 3.14445 12.7977 27.9672 4.00115 26.5743 379.7B7 1.79743 (nS/mL) nmmmmmm 3.14(M) 12.0 21,0 4.00 25.6 _50 1.90 QC Flag Legend M - Compound response manually integrated. -j 'I 1 t .i !'.!":;]i .... 3M EnvironmentalLaboratory Page 170 of 27( Report E02-0443 . _ Tenn. River Valley Samples $ 3M Environmental Laboratory Page 171 of 276 Report E02-0443 ]_ata File: _EtstaPie_tarlet_chem_dudejr.i_DO2OBi2A.b\I)UgEO071.9 3 PFOA (413) 9,0_ 9.0-." 7.0:. 6.0_ Ion 41300 m 54..0i_o v 3.0-:" >" 2.0i 1.0i 3.6o 3.8o 4._ i.'_ 4".'4"0 H_n 4 F0$_ (499) _..8" Ion 498.00 _ t,4" 1.2" "'4 i i0..O9": 0.4:. 0,2" 4,40 4.t= 4,90 5,00 5,20 Htn 5 PF0S (499) i.2 ._ _ 'i _..0" ! 0,8_ i _ 0.6". !I _ o.4: o.2_ _ J tA _.'_ ,_._ 4.'_ :,.'4_:I.'_ Hin . _ Tenn. River Valley Samples Pae 3 3M Environmental Laboratory D_ 177 _f 97_ ReportE02-0443 . _ Tenn.RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D0208"f2A.b\DUDE0078.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0078.D Lab Smp Id: 38033 Inj Date : 13-AUG-2002 01:34 Operator : mla Inst ID: dudejr.i Smp Info : 602-0443-38033; Misc Info : Water Samples; non-GLP; 6/20/02; OK Comment : Method : \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date : 27-Aug-2002 14:06 dudejr.z Quant Type: ESTD Cal Date : 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle: 27 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub _ds w_=z=R==mRm_==m=mlms_=msmM I PPBS (29%) 2 PPHS (399) 3 PPOA (413} 4 FOSA (496) S PFOS (499) QUANT SIO RA58 Jm=n 296 29% 296 399 399 399 413 466 469 RT _=_m 3.360 3.310 3.818 4.058 3.012 3.969 4.GIG 4.796 4.194 UXP RT m_n_=mR= 3.394 3.354 3.364 3.364 3.761 3.791 3.962 4.761 4.160 DLT RT RESPONS_ m_m=m_m= _--_m...s -0.034 26600 -0.184 0,424 4225 1671 0.664 0.021 634 $685 0.170 0.026 543_ 115_7 0.026 S467 0.034 3506_ CONCENTRATIONS ON -COL_R4N FINAL (ng/mL) =.===== (_g/mL) =_===== 0.45093 0.451 $03.706 504 S03.796 504 503.832 0,16974 504 0.170 0.16213 0.20121 0,162 0.201 0.17456 0.274 0.20349 0.203 3M Environmental Laboratory Page 173 of 276 Repod E02-0443 - Tenn. River Valley Samples Data File: \_Et.starl_et\target_hem\dudejr.i_lO20812R.b%DUgEOO78,D 2.0_ t.9: 1.9! 1,7t.6: 1.5! 1,4_ 1.3" ^ I.2! %_Ets tar_et%t aPget \ohem_k_ej r. |xJ)O20812R, b%DUDEO078. D t.0" >" 0.9- ,_ o.a-: 0.7: 4 Pa[e 2 0.2 .... 0.. | .... 1.0 e .... _.s m .... 2.0 | .... z.5_'; i ............ _..s..4..0.4...5.....0.5....5.."_....0.._....s._.'.;._:d 8.0 b .... a.s = ..... i'_" qtn I PF]BS(299) lo_ 29900 4.e" ;_ 4.4- _; 4.0" :! 3,6" 3.2- w ' _ 2.4-" _: / : 1,2 .8ii i *., ..o i..* 2.4 2.8 3.2 3.6 Hin i. *. 4.0 2 _ (3'_)) Ion 3_.00 m_h i _.4" _ "' ":'.".=.. t.0" >. 0.8: .'i ) 3.40 3.60 3.80 H|_ 4.00 4.20 3M Environmental Laboratory _ ,-_ _ "_-_ Report E02o0443 . _ Tenn. River Valley Samples l_t,a F_,te: \_Etst, arl:et_.tarl;eb%ohem_,dudejP.i_])O208_.2A.b\DUDEO078.9 3 PFOI_(43) Ion 43.00 o z.4- It " 2.0" t.6-: ;W 2,i..02_; t o.a-.: \ o.+-3_._6o3.+04.,.-o-_o4..,2._o+.,._. o H_,n 4 FOSA (498) I =-,i Ion 490,00 _- I .00- "4" o+LJ VL Io.,o4 iF I_.Toit 7o. ._i/ 0.40i I 5 PFOS <499) Ion 499+00 m 4.5_ 45..00-__ I/ i3.5i 1_ >- 2.0! to0-.; i 3.80 i .o- 4,00 Htn i.-. 4,20 i . i 4,40 4,60 Pal_e3 i .,.+ ;2.:J:"; "'-"' i:'" _M I_nvironment_l Laboratory _=,_o _-t_ r,_'_R i Report E02-0443 _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0080.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory Data file E02-0443, Tenn. River Valley Samples : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0080.D Lab Smp Id: 38034 Inj Date : 13-AUG-2002 01:57 Operator Smp Info Misc Info : mla : E02-0443-38034; : Inst ID: dudejr.i Water Samples; non-GLP; 6/20/02; OK Comment : Method : \\Etstargetktargetkchemkdudejr.ikD020812A.b\D020812A.m Meth Date : 27-Aug-2002 Cal Date : 12-AUG-2002 AIs bottle: 28 14:06 dudejr.i 16:13 Quant Type: ESTD Cal File: DUDE0027.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Coapounam mmmmn_mRmmmmmm=mmmummmmmmm 2 PPBS {299) 2 PPIf_ (399) 3 PI_OA (413) 4 O8A (498) 5 PPOS (499) Qt_NT SIO 14A_S _._m 299 399 413 498 490 499 RT EXP ET m==m mm_m. 3.401 3.812 4.010 3.394 3.791 3.982 4.796 6.0_0 4.194 4.760 4.768 4.160 DLT RT m_m_mm.. 0.007 0.021 0.028 0.028 0.322 0.034 RESPONSE ==mm..m= 28016 |673 17031 6747 276 51049 CONCLWTRATIONS O_- COI;m4N FINAL (ng/mL) _e..=_. (ng/mL) u=mm_=. 0.S0070 0.S01(M) 0.26104 0.50603 0.261 0.556 0.21607 0.00294 0.216 0.00294 0.71127 0.711 QC Flag Legend M - Compound response manually integrated. I .i 3M EnvironmentaLl aboratory Page 176of 276 Report E02-0443 , _ Tenn. River Valley Samples "4 Data File: %_E_s_l;et_tael;et_chem_dej,.i\l)o2oai2A.b_,DUDEOOSO.D 4.0" 3.8" 3.63.4 i 3.2-: 3.0_ 2.82,6! 2.4_ \_Et st arget%t ar_et _,che_\dudejr. i _,DO20812Ab.%I)UDEO08D0. z.zz.o. :)- 1.8, t.S-: t.4- Page 2 i 0.8-" 'i i 0.- 0.4-" i 1.o- .... , .... , .... m .... I .... o .... | .... , .... , .... i .... , .... , .... = .... i .... , .... | .... , .... o .... , .... 0.5 1.0 1.S 2.0 2.5 3.0 3.5 4.0 4.5 5.0 6.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 Mtn I PF_S (299) Ion 299.00N : 9.o- _- o e.o-: /_ r; /\ t s,o-: : _ 4.0" 2"o I // _-_- - 1,0-."._.j.. , . . . , . . . , . .. , . . . 2.4 2.8 3.2 3.6 4.0 Ntn 2 PR4S (399) 1on 399.00 i 3.3:\ II i 3.o" Z.4" !_.'_;L (_._.,..._; j;.:;.. _ _..5! $.2". , . . _ . . . , . . o , 3.40 3._|n3.80 4.00 4.20 3M Environmental Laboratory _,_ 17"r ,,_ o-_ Report E02-0443 Data File: %%Etstarl;et%tar'Eet\che_%dudejr.i%DO20812R.b_DU])EO080.]] 3 PFO_ (4t3) ,i 4.0,_ 3.6- 3.2- ff Ion 4i3.00 o 2.4" z.a" 2.0 i :J.o2_ t.6,:_ . o i - . o - - u - i - 3.60 3.B_|r14.O0 4.20 4,40 4 FO_ (498) Ion 498.00 r_ : ' i it ' .i _..0" 0.9-'." =.i" / 0.6" 0.5 i - i * i - o .- 4.40 4.60 4.80 Hin o *i o 5.00 5.20 5 PFOS (499) Ion 499.00 9.0- a*i ,e. 7.0" 6.0" 5.0i 4.0-" :%o _.0" . . , . . . , . . . , 3.80 4.00 4.20 Mtn 0- , 4.40 4.60 . - Tenn RiverValley Samples Pal:e 3 :::_'C:, _,,_!/O:::i'.iaina] ReportE02-0443 IIII I . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0084.D Report Date: 27-Aug-2002 14:11 Page 1 3M Environmental Laboratory Data file E02-0443, Tenn. River Valley Samples : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0084.D Lab Smp Id: 38037 Inj Date : 13-AUG-2002 02:41 Operator : mla Inst ID: dudejr.i Smp Info E02-0443-38037; Water Samples; non-GLP; 6/20/02; OK ', Misc Info : Comment : Method Meth Date Cal Date : \\Etstarget\targetkchemkdudej : 27-Aug-2002 14:06 dudejr.i : 12-AUG-2002 16:13 r. ikD020812A.b\D020812A.m Quant Type: ESTD Cal File: DUDE0027.D Als bottle: Dil Factor: 30 1.00000 Integrator: Falcon i: Target Version : 4.12 Compound Sublist : all. sub _I C==_=p=o=u=n=d=s================== I PFBB (299) 2 P_ 3 PPOA (399) (413) 4 _O_SA (498) S PPO,S (499) QUANT SIG M,_ nunn 299 399 423 498 499 ==R=T. o=E=X=p=w=R=T 3.253 3.805 4.010 4.796 4.188 3.394 3.'/91 3.982 4.768 4.160 ._DII ,T===R.T= -0.041 0.014 0.028 0.028 0.018 RIIInl_llUSPOMSE 32546 12978 14081 6547 43651 CONCB_T_RATI ONS ON-COLUMN PINAL n(llll=nX g/mL) 0.6S999 0.39367 0.36547 0.20948 0.47606 Il{lnllnng/mL) O.G60(M) 0.393 0.365 0.209 0.476 QC Flag Legend M - Compound response manually integrated. 3M EnvironmentalLaboratory Page 179of 276 Report E02-0443 . _ Tenn. River Valley Samples Data File: _\Etstarget_tarfet_ohe_dudejroi\DO20812A.b\nUDEOOa4.n Pa_e 2 4.6= 4.44.2" 4,0! 3.e3._,. 3.4! 3.2- "<Ill 3.0i 2.g" i2.,2 IIII \_Etsta_ret%t=r_et_he_\dudejr.i%I)020gi.?b_\I)UI)EO0_64 'I-ll t..82 1.6" 1.4" 1.2i i.OJ ? 0.4-: O0..2Gi-'_ 0,5 i.O l.S 2.0 2.6 3.0 3.5 4.0 4,5 5.0 5.5 6.0 6.5 7.0 7.6 8.0 8.5 9.0 t4*n 2 PF3S (.2c_) Ion 299.00 _, e'i I1" _.o" _| ' i ] 6.0 ! 5.0_ / xtI 4.0- 3.o" . 1,o2._._4,,_J2....8.....3..._ 3.6i ...4....0 H|n 2 _ (399) _ Ion 3__.00 ; a.9-\ ii' 3_'.,.'o__-: ,",_'_-. I_I= t,8: 1.5" v 2_..,2t_-" __c.._._ _,; ..3...G..0.....3...8.0.. 4.00 4.20 II|n c,:T_a_ctC"oa;.-vo/.zC_/._iraz,_- 3M Environmental Laboratory o_ __ _ 9=_ Report E02-0443 Data File: %%Etstar1_et_tarEet%oh_m%dudejr.i\DO20812A.b%I)UDEOOB4.D 3 PFCA (413) 4.5: 4.2- 3.9; 3._" p, _.o: 2.4J 2.1" 2t..e7:-: Ion 43._ o IL o II _ 1.2: '"i._-_ 4 FOSA (498) Ion 498..00 e,,.. _1 ,', iO_ o.9! to.2" .8i '7"= o.,_!'_ 0.s__ / I I/ / I 5 PF'OS (499) e.o" 7.0" 6.0" I_ 499.o0 .,. T 5,0: 4.0: _" 3.0 t_0: . . , . . . , ...... 3.80 4.00 4.20 Mtn ,. . . , . 4.40 4.$0 . _ Tenn. River Valley Samples Page, 3 $ 3M Environmental Laboratory Dp,_..I _1 _f 9"7_ Report E02-0443 I I . _ Tenn. River Valley Samples Data File : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0086.D Report Date: 27-Aug-2002 14:12 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0086.D Lab Smp Id: 38038 Inj Date : 13-AUG-2002 03:03 Operator Smp Info Misc Info Comment : mla : E02-0443-38038; : : Inst ID: dudejr.i Water Samples; non-GLP; 6/20/02; OK Method : \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date : 27-Aug-2002 Cal Date : 12-AUG-2002 AIs bottle: 31 14:06 dudejr.i 16:13 Quant Type: ESTD Cal File: DUDE0027.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub !_{ Compound= mnmmm._mmmmmmnmmmmmmmmn 1 PB8 (299) 2 PFH _= (399) 3 PPOA {43.3) 4 PO_A (491) S PFOS (499) ou_rr szG MASS mmmm 299 399 41% 4Si 499 RT mmmm 3.3S3 3.812 4.003 4.790 4.108 gXP RT mmmmmmmm 3.)94 3.701 3.9K2 4.788 4.160 DLT RT mmmnmmmm -0.041 0.021 0.02_L 0.028 0.028 RESPONSE SmmmmmN 3499E 11214 3.S130 2452 44191; ONCEZrn_ATZONS o.-coLu_. Pzm._ {ng/mL} mnaBmmn (ng/=n) mmmnmmm 0.74264 0.24701 0.4_37_ 0.10"/54 0.49338 0.743()1) 0.247 0.434 0.108 0.493 i QC Flag Legend M - Compound response _nually integrated. -I .t i ExacCt opyof0rig,"na_ 3M EnvironmentaLl aboratory Page 182 of 276 Report E02-0443 . _ Tenn. River Valley Samples r.__ ])ata File: _%EtstaPget%taPi;et_:_he_dudejr.l%D0201_2A.b%gUl)E0086.]} 4.24.0, 3.S" 3.63.43.2, 30i 2.8! Z.6-" 2.4! \_Etst_PI;et%t_lrget%ch_JdeJ r. L%_020812Rb. _])UDE0086D. Pace 2 1.Bi I.- v 21.04" _ _..OJ 0.80.6 ............................. 0.5 t.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 Htn i PFBS (299) Zon 29900 ,.oi ,.All _ 4o0_ > 3.0 A/v_r _.o:,_./.]............. 2.4 2.8 3.2 3.6 4.0 Hi. 2 PFHS(3_) Ion 399.00 : 3.6i\ + 2.42 1.5" 0.92 i I i i i 3.40 3.60 3.80 4.00 4.20 H_n t!_ct Copoy_Or;.gi_m_ ++ 3M Environmental Laboratory D_ + o-) ^, "_',r Report E02-0443 I Dat, a Fire: ,_%Et,starget%tar-et_che_udejr.t%DO20812R.b%_J_O086.D 3 PFOA (413) ion 413.00,1. z.9- II 36_. 3.0-: 2.7" 2.4" 3.3d ._ /l 10.92-"_ i t - i *i t o 3.60 3.80 4.00 4.20 4.40 H_n 4 FOSA (496) ton 498.00 .- 800" " _J _so-_ _o" 45o 4oo_ i 4.40 i . . m 4,_) 480 H1n - i I !5.00 _5,20 5 PF06 (499) Ion 499.00 ; e.o" I s.o" ; 7.0- , 4.0-_ I ,,e i 2.0!_.._ , i , . . i 3.80 4.00 4.20 ,, H;_n .. |. 4.40 . _, 4.60 : . _ Tenn. River VaUey Samples Pal:e 3 ':'__cCcop;o, _Or!gina! 3M Environmental Laboratory P_n= 184 of 77_ ReportE02-0443 . _ Tenn.River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0127.D Report Date: 29-Aug-2002 07:12 Page 1 3M Environmental Laboratory Data file : Lab Smp Id: Inj Date : Operator : Smp Info Misc Info : Cogent : Method : Meth Date Cal Date : AIs bottle: Dil Factor: Integrator: E02-0443, Tenn. River Valley Samples \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0127.D 38028 13-AUG-2002 10:35 cmc E02-0443-38028; Inst ID: dudejr.i Water Samples; non-GLP; 7/17/02; OK \\Etstarget\target\chem\dudejr.ikD020812B.bkD020812B.m 29-Aug-2002 13-AUG-2002 41 07:08 dudejr.i 06:44 Quant Type: ESTD Cal File: DUDE0106.D 1.00000 Falcon Compound Sublist: all.sub Target Version: 4.12 Q,..m,_sza CO_TIO_ O_-COLUm_ _Z_ _ Compoun_ =mmmmmmm_m=mm=mmmmmmmmm=mm 1 PFB8 (299) 2 PYHS 3 PpOA 4 rOSA S PPOS (399) (413) (49_) (499) N_._8 mmm_ 299 299 299 39_ 399 390 399 413 490 499 RT BXP RT m_=m mm_.m_m 3._00 2697 3.073 3.777 4.085 4.249 3.777 3.962 4._41 4.140 3.394 3.394 3.394 3.394 3.394 3.394 3.791 3.983 4.76_ 4.180 DLT RT RESPONSB _mmm=mmm mmmm==m= -0.006 -0.097 -0.321 0.303 0.691 0.8S5 -0.014 -0.030 -0.927 -0.030 195308 963 9274 8460 602 4]9 7874701 3048302 0025349 ?827644 (ng/_) mlmm.mm 2926.60 2935.68 293S.29 2935.33 2935.G9 29]5.70 392.569 388.428 302.105 38_.783 (ng/_) mm_=m== 2930 2940 2940 2940 =940 2940 392 ]80 _02 362 '"'_?."-5._(;// :. ,_,'_:.::j, 3M EnvironmentalLaboratory Pa_e 185 of 276 Report E02-0443 . _ Tenn River Valley Samples 3M Environmental Laborator_ Paae 186 of 276 Report E02-0443 . _ Tenn. River Valley Samples Data File: _Etst._*getStarget\cheM\dudejr.i%1)O208123.b_DUDEO127.D 3 PFO_ (4t3) Iors 4_.3.00 7.06.05+0! 4.0x 3.0" _" 2.0! i.O: -.,3.60 I , 3.80 4.00 Hln 4 FOSA(4_8) Ion 498 O0 . ,.,., 4.20 .I 4.40 t.2- _..O_ 0.6i 0.8- > 0.4- 0.2- : = I. i ...... 4.40 4.(;0 4.90 Hip I 0 _ D 5.00 5.20 5 PFOS(4_) to2_ 4.0" ion 499.000 0.6: i o.6- _- 0.4 i 02" :....!............_.,_. 3.80 4,00 4.20 4.40 4,60 Pal;e 3 3M Environmental Laboratory Paoe 187 of 276 Report E02-0443 . + Tenn.River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D0208f2B.b\DUDE0133.D Report Date: 29-Aug-2002 07:12 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812B.bkDUDE0133.D Lab Smp Id: 38036 Inj Date : 13-AUG-2002 11:41 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443-38036; Misc Info : Water Samples; non-GLP; 6/20/02; OK Comment : Method : \\Etstarget\target\chem\dudejr.i\D020812B.b\D020812B.m Meth Date : 29-Aug-2002 07:08 dudejr.i Quant Type: ESTD Cal Date : 13-AUG-2002 06:44 Cal File: DUDE0106.D Als bottle: 43 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist: all.sub Compounds mm.mmmmmmmm_mmmm_nmmm_mmml I PPBS (299) 2 PPHS (399) 3 pPOA 4 pO.SA 5 pFO8 (413) (490) C499) QUANT BIG M_SS mmmm 299 299 389 299 299 399 413 498 499 499 RT mmmm 3.38t 3.073 3.777 4.085 4.242 3.771 3.962 4.735 4.133 3.832 gXP _T mmmmmmmm 3.394 3.394 3.394 3,394 3.394 3.791 3.9D2 4.762 4.160 4.160 DLT P:_ mmmm.mnm P_Lq_O_S_ .mmmmmmm -0.006 -0.321 0,383 0.691 0.848 2020S3 26005 9S00 820 817 -0.020 -0.020 -0.033 -0.027 -0.328 6071912 3927038 0558553 7890357 906 CONCRNTRATZONS ON-COLUMN FXNAL (ng/-t.) mmmmmi= (ng/mL) ._mmmmm 2926.29 2934.08 2935.28 2935.68 2935.60 2_30 2930 2940 2940 2940 404.870 398.487 324.535 365.265 3071.25 405 398 324 3ES 3070 3M Environmental Laboratory P_oe 180 of 276 al Report E02-0443 I I I . _ Tenn. River Valley Samples 3M EnvironmentalLaboratory D_,,,__o _ '_7_ ReportE02-0443 I I . _ Tenn.RiverValleySamples Data Fi|e: ',.'_Etst,aP[et\t, ar'et"_J'mm\dude.jr.L_._20812).b\_DE01339 3 PFOR(43) Xon 4"13.00 7.0:. G.o_. 50-: <_4.o4 v . > 2.o" 1.0- 3.6 3.80 4. Htn 4 FOSR(498) 4.2 4.40 1.2- : 1.02 I^ 0.8: _ ][on49e._ , 0.6-" ;'l v >- 0.4" 0.2- I I * 0 - i , i * - I 4,40 4.GO 4.80 B.OO 5.20 5 PFOS (499) I lob 499.00 1,2- _i 1.0_ ".1 t i o.8- ':_ >,, 0.42 0.z" : || 3.80 i II 4.00 HArt 4.20 I i #/ 4,40 460 t Paire 3 _L-- J ..J_._ 3M EnviTonmental Laboratory D,,,o 4 _n _c ,_-_ ReportE02-0443 .. _ Tenn.River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D0208i2B.b\DUDE0136.D Report Date: 29-Aug-2002 07:12 Page 1 3M Environmental Laboratory E02-0443, Ten n . River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0136.D Lab Smp Id: 38040 Inj Date Operator : 13-AUG-2002 : mla 12:14 Inst ID: dudejr.i Smp Info E02-0443-38040; Misc Info : Water Samples; non-GLP; 6/20/02; OK Comment : Method Meth Date Cal Date : \\Etstarget\targetkchem\dudejr.i\D020812B.b\D020812B.m : 29-Aug-2002 07:08 dudejr.i Quant Type: ESTD : 13-AUG-2002 06:44 Cal File: DUDE0106.D Als bottle: Dil Factor: 44 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Coipoundm _===usauam==m.w==mmmi==is= 1 pP1BS (299) 2 PFHS (399) 3 pPOA (413) 4 pO.SA (498) 5 PFOS (499) QUANT SIG MASS ==n= 299 299 299 299 299 399 423 498 499 RT sl== 3.3t7 2.936 3.073 3.832 4.023 3.777 3.961 4.741 4.132 EXP RT ====m=== 3.394 3.394 3.394 3.394 3.394 3.791 3.982 4.768 4.160 DLT RT i======m -0.007 -0.4S8 -0.321 0.436 0.629 -0.014 -0.021 -0.027 -0.028 RESPONSE m_====_= 200230 5425 13185 10649 405 824;279 3997548 7955852 7760025 CONCENTRATIONS ON- COLUMN (ng/mL} ==mR=m= 2926.37 2935.47 2035.11 2935.23 2935.70 410.87S 407.5B9 299.20S 358.040 FINAL (ng/mL) =1===== 2930 2940 2940 2940 2940 411 40Q 299 358 3M Environmental Laboratory Page 191 of 276 Report E02-0443 . _ Tenn River Valley Samples 3M Environmental Laboratory P_e 192 o_ 276 Report E02-0443 . _ Tenn. River Valley Samples ._ Data Ftle: \_Et, st,aPIl;et\taPet\ch_ludejP.t%DO20812]B.b_DUDEO116.g 3 PFO_ (4_3) Ion 413.00 7.0" 6.0-: _ 4.,! 3.0- _" 2.0- _..0 . , . - Ii - i . . , o , I 3,60 3,80 4.00 4.20 4,40 Hin 4 FI_3R (498) Ion 498 O0 t.2- '_ i i.14 _.o_ '; 0.9_ 0oa_ 0,7-.' ; o.6_ O.B_ 0.4_ 0,3_ 0,2! 0.t" ; .. .. 4.40 i , . . . , . . . , , 4.(=0 4.80 5.00 . | .I 5.20 5 PFOS(499) | t.2_ t.t" ]on 499,00 0o9_ e _, 0.6; >- 044 .3_ 2._ 1 i ! | -, - _ - t t - . f L 3.80 4.00 4.20 4.40 4.60 Pace 3 F;:o_Co;::-:::..':._.: 3M Environmental Laboratory Pane t93 of 276 Report E02-0443 I I . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY034.D Report Date: 19-Nov-2002 14:49 Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\IO21112.b\ITCHYO34.D Lab Smp Id: 0443-WB-I Inj Date : 12-NOV-2002 13:40 Operator : mla Inst TD: itchy.i Smp Info : E02-0443-WB-I; Misc Info : Water Blank; MeOH Extract; 21 Oct 02; MLA Comment : Method Meth Date : \\Etstargetktargetkchem\itchy. : 13-Nov-2002 09:16 itchy.z Cal Date : 12-NOV-2002 12:14 AIs bottle: 21 Dil Factor: 1.00000 i\I021112 .b\I021112 .m Quant Type: ESTD Cal File: ITCKY026.D Integrator: Falcon Compound Sublist : all. sub ._ Target Version: 4.12 C_p_n_ . ===== ===== i===_==n===n= 1 PgB8 (299J 2 P_ 3 pPOA (399) {413) 4 FOSA (498) i 5 pl:os (499) QUANT Big MASS =m 29.9 299 299 399 413 413 480 499 RT 3.421 3.252 4.129 3.840 4.03,9 4.348 4.867 4.209 IXP RT 3.422 3.422 3.422 3.830 4.020 4.020 4.867 4.199 DLT RT = == -0.001 -0.170 0.707 0.010 0.019 0.328 0.000 0.010 RESPONSE === == 37874 7026 7365 2541 13412 10274 1927 78922 CONCSNTRATIONS ON- COL_N FZNA/., (ng/-r.) ======= (ng/mL) = ===== 0.$5035 933.500 933.490 0.:L3306 744.874 748.050 0.5.50 933 933 0.133 745 745 0.17214 0.172 1.09119 1.09 i .1 :_.1 ._...'. "1 3M EnvironmentaLl aboratory Page 194 of 276 Report E02-0443 . _ Tenn River Valley Samples 3M Environmental Laboratory Paoe 195 of 276 Report E02-0443 : ' ! :I ' ii:t, ; i i ; ' ::J ,.._ : : Datl Flle_, '.,_Et;star'l;et\t.ar'l;et',_che_t%ttah_.t\IO2:.l12.ob\ITCHYO34.D 3 PFOR (413) Ion 4:/.3.00 2.42,22.0" :L @-." i 1.4-.: _.2" ioO- o.e4 0.6_ 3.60 3.80 4,00 4,20 4,40 H_n 4 FOTg_ (49a) Yon 49a,00 78o- ,; , /[ 7zo-.' I_ ;'5 l/ _,i ,a 6,o_ / t / Y =:,J ....... 4.,4o.,Io;o,.o_,.2 @ PF'OS (499) 'l ,,O_ 0o9_ 0,8-: o.7_ Ion 499.00 _v 0o.4-.s: >" 0.34 0,2_ o._'_ = = . =-.-i..t 3.80 4.00 4.20 4.40 Htn 4,60 . _ Tenn. River Valley Samples Pace 3 3M Environmental Laboratory Paoe 196 of 27_; ReportE02-0443 . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\iTCHY035.D Report Date: 19-Nov-2002 14:49 Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\iTCHY035.D Lab Smp Id: 0443-WB-2 Inj Date : 12-NOV-2002 13:51 Operator Smp Info Misc Info Comment : mla : E02-0443-WB-2; : : Water Blank; Inst ID: itchy.i Me0H Extract; 21 Oct 02; MLA Method : \\Etstarget\target\chem\itchy.i\I021112.b\I021112.m Meth Date : 13-Nov-2002 09:16 itchy.i Quant Type: ESTD Cal Date : 12-NOV-2002 12:14 Cal File: ITCHY026.D AIs bottle: 22 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 i ,= _ Compounds ==mmm_===m=.=mmmmmmmmmm=mm 1 PPB8 (29S) 2 PP_ (399) 3 PFOA (433) ; 4 FO_L%, (4SS) ! S PP08 (499) Q_Ai_'T BZG MASS =m=. 299 2S9 25S 399 3SS 413 433 4gs 499 RT EXp RT DLT RT R_NSH m_mm .mm_m==w mmn_mm== _._m_=== 3.4_1 3.2S2 _,11_ 3.830 3.491 4.029 4,_48 4.S07 4.219 3.422 3.422 _.t22 3.830 3.030 4.020 4.020 4.tG7 4.199 -0.011 -0.170 0.E$? 0.000 -0.339 0.009 0.320 0,000 0.020 32544 5958 3285 3G28 1344 14SS2 12065 2tS_ 42341 _N_NTRA,TZONS ON- _]bD1R_ PZNAL (_/_) =.==_i= (_/mL) mw===mm 0.3972G 933.530 933.607 0._5042 0.10734 0.04334 744.949 0,18434 0.23630 0.397 234 S34 0.156 0.107 0.0432 745 0.114 0.236 '1 3M EnvironmentalLaboratory Page 197of 276 ReportE02-0443 ii ii I I . _ Tenn. RiverValley Samples _ata Filet %%EtstarEet%tar=e_-%:he_\itol_jot%][O21112.b\1TCHYO35oD 3.83.6: 3.4-. :3.2_ 3,0_. 2.8;. 2.6_. 2o4_ 2.2-_ 2.0 i iv 1.8: >- \_l[f, st, ar_et,\t_" [et.%che m%i_,Gh_J,i %Z0_-1_2. b\ I TCHY035. D Pale 2 _ .4_ _!!! i ; : , ' i :LoO-" 0.8O.G.-_ 0.4,_ o.2-__,J,k, _................................................................................... 0.5 :1.0 t.5 2.0 ::'.5 3.0 3.5 4.0 4.5 5.0 15.5 6.0 6.5 7.0 7.5 8.0 B.5 9.0 Hip :L PF]BS <2_)) 5.2 i 4.e- 4.4-." z.6_ 2.8-: Ion 299_00 ....... 2.8 3.2 3.G 4.0 4.4 2 PFHS (3_9) ]on 3c_ o0 i.oo,:" /" o,oi =t : o._ I} " / ) 0.70-" _" o,,! > o._o;, k | _ ! _. I I / _._ - _._$_._ "_,._ ;_._- , , _tn *J:._a.(Cop3 l: '3_!;;!n_! - ";"* 3M EnvironmentalLaboratory Paoe 198 of 27_ i ReportE02-0443 Data File: _\Etstarget_tarEet_che_itch_J.i%IO21112.b_ITCHYO35D 3 PFOR (413) ZQn 4:1.3,00 z._" _. o 22-: [/ _r t.62 1o44 1_.2.e" 4 ,, 1z,.Oo-_.': /_,. _ _.'+__o_ ;,._ _._ ;,.,,+_ Mln 4 FOSA 49e) 880 Ion 498.00 );! > +40" 6oo" _, _o_. 5 PFOS (499) _._i _ _l Ion 499 O0 _h 1 4.4: II i: _"+" t . _ _:.4 -" : _. 2,0 3,80 400 4.20 4,40 4_ tii,_ i P II I . _ Tenn.RiverValleySamples ._ Pate 3 _/,actCopyof Ori.qin_! 3MEnvironmentaLlaboratory Page199 of276 Repo_ E02-0443 . _ Tenn. RiverValley Samples Data File. \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY038.D Report Date: 19-Nov-2002 14:49 Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY038.D Lab amp Id: 0443-38044-1 Inj Date : 12-NOV-2002 14:23 Operator Smp Info Misc Info : mla : E02-0443-38044-I; : SL-!; MeOH Inst ID: itchy.i Extract; 21 Oct 02; MLA Comment : Method Meth Date : \\Etstarget\target\chem\itchy. : 13-Nov-2002 09:16 itchy.i i\I021112 .b\I021112 .m Quant Type: ESTD Cal Date : 12-NOV-2002 Als bottle: 25 12:14 Cal File: ITCHY026.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 Compound Sublist : all.sub ;_ Compounds =SSS = Smm. W iiimmmnmms l m 1 PFBS (299) ; 2 PPHS (]SS) 3 PPOA (413) 4 POSA 5 PPO8 (498) (499) QUANT SIG MA_S i=a 299 295 299 399 399 413 413 498 499 RT EXP RT DLT RT _=mm i=m _==m _=.mmwmu 3.$II 3.422 O.Oa9 3.9"}0 4.309 2,422 3.422 0.549 0.887 3.840 3.432 3.830 3.530 0.010 -0.398 4.040 4,020 0.020 3.701 4.020 -0,219 4.187 4.219 4,867 4.199 0.020 0.020 RBSPONSB ==_===== 303==59 2593 4148 122635 15909 295590 8211 1250415 2785277 CONCENTRATIONS ON -COLDMN FINAL (ng/mL) _=m==_. 10.5978 93"%. 52 ") 933.582 2.71999 0.40492 16.1949 745.166 29.6711 67._562 (ng/IL) ==Bm=ss 10.6 9"_4 934 2.72 n.4Q5 16.2 745 29.7(R) E?.6(M) i:i QMC - FlCaogmpouLnedgend response manually integrated. .:_ :t 3M EnvironmentalLaboratory Paoe 200 of 276 Report E02-0443 II II . _ Tenn. River Valley Samples _,! i :i I !i ' :::i Data File: %%Etstarl;et%ta*get_.o_\Itch_.l\lO21:Li2.b\ITCHYO3B,D 4.6" 4.4" 4.2-: 40-_ 3.e" 3.63.4-" 3.2-_ 3.0" 2,8-_ 2.6" 2.4-.: 2.2" >. 2. o -:. i.a" \\Etstarget%tar_et_ohe_\itoh_. i%I021112.bXITCHY038, PaEe 2 1.4-_ _ i o.a-_ 0.4" / 0.2! ,,_1,._,_ .... , .... , .... , .... , .... , .... , .... , .... | .... | .... | .... , .... , .... , .... 1 .... , .... u .... | .... , .... 0.5 i.O t.5 2,0 2,5 3,0 3.5 4.0 4.5 5,0 5.5 6,0 65 7.0 7.5 80 B.5 9.0 Hin i PFBS (299) ii!- i.s: "" ^ _C.4" Ion 299.00 k / 1 o I1 _..0-." F\ 06" .4- o.2i___t | . , .. ,-. 2.8 3.2 3.6 ,, tS_n 2 Fq:HS (399) _ iv , *, 4,0 4.4 Ion 3_.00 4 2.6" _ 2.2- .... _..... i i1.8.4"" >" 1.2" ,e 0-ai"=C::::::::_ 3.40 3.00 3.80 4.00 Hlq ,_ 4.20 _;_ .,. e 3M Environmental Laborato_ p=_,= ?n_ _ ?_ Report E02-0443 i i :".,i . _i Data File: %_EtstaPCet%taPcet_hc_%itch_j.i%IO21i12,b\ITCHYO38.J3 3 PFOR (413) 5.2" Ion 4t3.O0 4.4_ 4.0" 3,6-." 2.8_ i 3.2 -." v 2.4-_ 1,6-.' , i.2- m j o.s4----J-2_J, i , = - i - , . i . . 3.60 3.80 4.00 4.20 4.40 4 FOSA (498) Ion 498. O0 v. i.e" /I '; 1.4" ! i.o: [_ v o.._"s_ ]/ 0,.42:; i I/ ! 4,40 4.60 4.80 5.00 5,20 H_n 5 PF0_ (47_) Ion 499.00 4.0- :3.63.2" 2.8" 4.4- ! 22.0.4" .G" I_ 0.0- 0.4._ f ./ - , , i i - | , 3.80 4.0g 4,L_ 4.40 4,60 Hr. , I . _ Tenn. RiverValley Samples Pace 3 3M Environmental Laboratory P_n= ?_ _ _'_ Report E02-0443 ,. _ Tenn River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY040.D Report Date: 19-Nov-2002 14:49 Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY040.D Lab Smp Id: 0443-38044-2 Inj Date : 12-NOV-2002 14:45 Operator : mla Smp Info : E02-0443-38044-2; Misc Info ; Comment : SL-1; Inst ID: itchy.i MeOH Extract; 21 Oct 02; MI._ Method : \\Etstargetktargetkchemkitchy. Meth Date Cal Date : 13-Nov-2002 : 12-NOV-2002 09:16 itchy.i 12:14 Als bottle: 26 Dil Factor: 1.00000 i\I021112 .b\I021112 .m Quant Type: ESTD Cal File: ITCHY026.D Integrator: Falcon Target Version: 4.12 Compound Sublist: all .sub i L I _il _4= IIIIIIII _ III I IIIIIIIIIII II 1 PI=B8 (299) 3 PI:HS (399) 3 ppOA (4139 4 POSA (498) 5 P1:'OS (499) QoJ_-s:xG #Ass IIII 299 299 299 389 399 413 413 490 499 _ IIII 3.432 3.970 4.309 3.040 2.432 4.040 3.711 4.887 4.219 _,XPP.T OnTRT _POLgS_ III I IIII llllll_= IIIIIIII 3.422 3.432 3.422 3.830 3,830 4,030 4.030 4,867 4.199 0.010 0.548 0.887 0.010 -0.398 _.020 -0.309 0.020 0.020 383608 2970 62861 118901 1387_ 2&000_ 9504 1351450 2885124 C_N(_IqTI_TZONS OH-COnUNN PX_UU, (nglu;..,) (ngI,,T-) III I=II IIIIII I 10,5904 933.645 1.36871 2.639:37 0.37(;75 14.1091 745.093 32.3550 70,2517 10,1; 934 1.27 2.64 0.377 14._, 745 32.4 70.2(N) QC Flag Legend IX M - Compound response manually integrated. :i ,,% ..-;.;i.......... :.. 3M EnvironmentalLaboratory Pa(_e203 of 276 Report E02-0443 Tenn River Valley Samples Data File: %%Etstar=et%tarEet_che_%itch_.i%IO21112.b%ITCHYO40.D 4.84.6" 4.4-: 4.2! 4.03.8: 3.6_ 3.4! 3.2" 3.02.8" 2.6! _%Etstam-_et\twr_et_ch_m_ itch_ i%Z021112.b% ITCHY040. B i 2.42-.' :- ZO _. 1.8! t..2" !t o.a" 0.6" 0.4" 0.2" Nln i PF_ (299) Zm Z99.00 ,.,i 2.0- J u ,,4 . _'_i l.4- J/ I_ o_ It1l , I, _- i."o{_ /f \_v"_ 1v12' ..,.. -_,z. "3:,.."4,o'.._, tt|n 2 PFHS (3e_) Ion 399.00 :' z.4" ;, ..; 2.2" ,,; 1.4" i.O_ _ k 3.,_, :a._o a.so 4.oo 4.zo Pale 2 F/_aCctopoyf Ori_;_.._; 3M Environmental Laboratory Page 204 of 276 Report E02-0443 , _ Tenn. River Valley Samples _ta FLIe: \_Etst, arl;ef,\f, arl;et'_che_,it, ch_.t%_O2_._.2.b\IT_Y040.9 3 PFO_ (413) 4,4" 4.03.6-." 3,2_ lor_ 4_.3,00 .o ,t 2.4" 2Z..Oa_- _.z" '; o.+'_ ,,_, i I .... 3.60 3,,8<) ioO0 4.'2() Htn 4 FOS_ (498) Ion 49a,oo =r_ i 4.40 i 2_..o.6-- . "L.4- ii _LO: _: i to..Za"- :" 00,..642:-"-." Ij I "'1 + + i - I 4.40 4.GO 4.80 5.00 5.20 5 PF08 (499) I Ion 499,00 I 44..40:" ; 3.z-: I 2.8- __ l i 22.04__ i l..Z-_ : 0.8- 0.4-:' ! J I | i . i I 3.80 4.00 4,20 4.40 4,60 Hin +i Page 3 ;:_ !: _.O'dfginP.l 3M Environmental Laboratory Page 205 of 276 ReportE02-0443 . _ Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY042.D Report Date: 19-Nov-2002 14:49 Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY042.D Lab Smp Id: 0443-38044-3 Inj Date : 12-NOV-2002 15:07 Operator Smp Info Misc Info : mla : E02-0443-38044-3; : SL-I; MeOH Inst ID: itchy.i Extract; 21 Oct 02; MLA Comment : Method : \\Etstargetktarget\chemiitchy. Meth Date : 13-Nov-2002 09:16 itchy.i Cal Date : 12-NOV-2002 12:14 Als bottle: 27 i\I021112 .b\I021112 .m Quant Type: ESTD Cal File: ITCHY026.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.12 J Compound Sublist : all. sub i i _ Compounds _lmmm=w.ummllnmm_mmm_mlm_= 1 PFT:tS 4299) 2 PIBHS 4399) 3 _VOA (413) 4 POSA S PPOS 4498) {499} QUANT SIG MASS _m= 29% 299 399 399 4_3 413 491) 499 RT BXP RT mm_m mtmmm_nm ].T,31 4.299 3.422 3.422 3.840 3.432 3.830 3 .1)30 4.040 4.020 3.701 4.020 4.J1)7 4.219 4.867 4.199 DLT RT RESPONSE m=mm_mm_ mllm==mm 0.109 0.877 482034 50026 0.010 -0.1)90 111724 19590 0.020 253343 -0.31_ 0515 0.g_0 0.020 i03_771 2109105 CONCSST_TIO_S 0N-COLUMN (ng/mL] _=m..mw 13.4094 0.09957 2.48445 0.49957 13.7201 74S. 149 24.4631) 50.3621 PINAL (ng/mL) _mm_..= 13.5 0.900 2.41) 0.500 13.7 74_ 24.54M) 50.4 QC Flag Legend M - Compound response manually integrated. 3M EnvironmentalLaboratory Page 206 of276 Report E02_143 II I I . _ Tenn River Valley Samples 3M EnvironmentalLaboratory Paae 207 of 276 ReportE02-0443 Data File: %_Etstaret_ta_Eet%chem\itch_.i%IO21112.b_ITCHYG42.D 3 PFOA (413) 4.4 4.0" 3.6" A 3.2_ Ion 4t3.00 ,t 22.4.s" - >. 2.0- o_ .24 ? o.e.:----.z=_, j , - * J - , * i , * 3.G0 3.80 4.00 4.20 4.40 Hi. 4 FO_I (498) ,o,4, ,8.o* i.4" 4 1.2" 't.O, _ 0,6 , 0.42":;.__ I/ I I - = , - , , 4.40 , 4.00 4.80 S.O0 15,,20 H;n 5 PFOS (499) Ion 499.00 0 2.7" 2.4, 2.1" i!t 3.0" I' ! 1i.2."8, 00..93"':, I * 3.80 -| 4._ .. - o* *4.20 Hlr_ I - i - - m 4.40 4.60 . _ Tenn. River Valley Samples Pace 3 :"_. "i ..... -/" "_" 3M EnvironmentalLaboratory P_=_ _C)8_f 77_, ReportE02-0443 | . _ Tenn. RiverValley Sampres Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY046.D Report Date: 19-Nov-2002 14:49 Page 1 39 Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY046.D Lab Smp Id: 0453-38045-I Inj Date : 12-NOV-2002 15:50 Operator : mla Inst ID: itchy.i Smp Info Misc Info : 802-0443-38045-I; SL-3; Me0H Extract; 21 Oct 02; MLA Comment : Method : \\Etstarget\target\chemkitchy. i\I021112, b\I021112, m Meth Date : 13-Nov-2002 Cal Date : 12-NOV-2002 AIs bottle: 31 09:16 12:14 itchy.i Quant Type: ESTD Cal File: ITCHY026.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist : all. sub :_ Target Version: 4.12 ",] ; CONCRMTRATI ONS i_ Com%pounclm mmm=mmmnm nlammmim.m mnNlmi um lm 1 _PBS (3599 2 PP'H8 (399) 3 PFOA (4139 , I 4 FOSA (498) ;u ;i 5 ];_0S (499) M/%_S mmmm 2gg 299 299 399 389 413 413 413 498 498 489 499 RT mmnm UXP RT mm_m_mm 3,412 ] .950 4.309 3.840 3.442 3.422 3,422 3.423 3.830 3.830 4.040 3.711 4.020 4.020 4.379 4.087 4.598 4.219 4.S60 4.020 4.067 4.867 4.199 4.199 DLT RT NmWm _n_ RESPONSE mmmmi.m_ -0.010 0.$20 O. 8117 0.010 -0.3BE 3252g4 2272 17131 13341 8750 0.020 -0.309 49046 9123 0.359 0.020 -0.269 0.020 0.369 7941 48310 r'L_ 418,JS4 11802 (ng/.L) .mnmnmn 8.81037 933.636 933.210 0.36520 0.26651 1.92925 74S,11S 745.181 1.24672 0.24"7_4 9.07817 1354.25 (.g/IL} nmmmmm. 1.8a 934 933 0.365 0.266 1.93 74S 745 1.25 0.26B 9.00 1380 .I ! 3M EnvironmentalLaboratory Page 209 of 276 Report E02-0443 . _ Tenn. RiverValley Samples 3M EnvironmentalLaboratory Paoe 210 of 276 Report E02-0443 Tenn River Valley Samples l_ataFile" _,_Etsta_&et_tar_et_he_ItohB.i_lO21112.b_ITCHYO46.D 3 RFOA(413) 1._; i.zsi 1.20" Ion 413.00 _ /I _ : : !:!,! ' "-] :i ,....: ': o.gs=; _ "'_i A o.8_ !\ 0..o,' / \ Ii _\ f1_ I1\ ,J \ il\J / "_ /I/ - 0 | t ,. B. --= 3.60 3.80 4.00 4.20 4.40 Htn 4 FOUR(498) Ion 498.O0r_ 7.5,: ( 7.o" I _,- __..o'"- == /f 0-4.5. ,; 1 L / :::i,4_40 4.60 4.80 5.00 5.20 Htn 5 PF(:_ (4cY)) 0.o _ _. Ion 499.00 "! l/ 4.0-: 3.0 2. / i*Oi D - o D | .-_ ;3.00 4oOONfl_.20 4.40 4.60 t Pa_;e3 .. ..... . ;.'_'._ . [,.-r_.;_] . ...... 3M Environmental Laboratory Page 211 of 276 ReportE02-0443 ._ Tenn.River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY048.D Report Date: 19-Nov-2002 14:49 Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY048.D Lab Smp Id: 0453-38045-2 Inj Date : 12-NOV-2002 16:12 Operator : mla Inst ID: itchy.i Smp Info Misc Info Comment : E02-0443-38045-2; : SL-3; MeOIt Extract; 21 Oct 02; MI_ Method : \\Etstargetktarset\chem\itchy. i\I021112 .b\I021112 .m Meth Date : 13-Nov-2002 Cal Date : 12-NOV-2002 AIs bottle: 32 09:16 itchy.i 12:14 Quant Type: ESTD Cal File: ITCHY026.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub i Target Version: 4.12 ! : ,ill Comi._d, + ills llmeimml llmmmmim nmmmm I pFIlS (299) 2 PI;'I_ t (399) 3 PFOA (41"1) 4 FOSA (498) 5 PO8 (499) ou,,u_ -zo ilksS wmmm 299 2_95. 299 399 3_9 399 413 413 490 498 499 499 _ ilXPliT i:)UiR' T itilSiOilsll + s Im IllS+Ill mmm+ IIii ilmmliml "1.421 3.422 -0.001 30101 3 . 9GO 4.310 "1, 422 3.422 0 . 5311 0.196 71119 12129 3.840 3 .&*.l 3.130 3.130 0.010 -0 ..115 11469 11109 4.029 3.830 0.199 10665 4.049 3.710 4.020 4.020 0.029 -0.310 602"11 11";54 4.1111; 4.617 4.06? 4.167 0.029 -0.250 46172 4067 4.229 4,199 0.030 22.194_ 4.561 4.199 0.369 6125 CONCBNTRATIONB o,-coLtm, Fz_ (.g/..+.) lillll+ trig/it+) lillli I i.29121 0.39 933 . 495 93 "1. 3"1.1 9"1"1 933 0.32491; 0.46772 0.325 0.460 0..1071;7 0.300 2.1:181;6 '745.135, 2.1;2 ")4.% 1.19716 0.22171 1.20 0.222 g.145"1_ G.G4 1254."17 1350 /,7.1il0+"<_- u...-+u. 3M EnvironmentalLaboratory Page 212 of 276 Report E02-0443 Tenn. River Valley Samples 3M Environmental Laboratory Page 213 of 276 Report E02-0443 98ta File$ %_Etsta_l_e_%targtt%ohem%itch_.i%IO21112.b\lT_YO4S.D 3 PFOA (413) Ion 413.00 5" " i.i -.' 110! O Jl_ I_ o_+ I.0.; '* ; ,d o.w_ _ o.es, r,; o.8o_ , .A 0.70 i ::_J...... 3.GO 3+80 t/ It I 1\ H/ ...... 4.00 4.20 /_ _.... 4.40 4 FOSA (498) Ion 4_.00 _. 8.0 i 6.0" i-i7.0" >-4,i0 ] ,1 /_ 3.o'_! 4.40 4.60 4.80 5.00 5,20 Mtn 5 PFOG (4c_) Ion 499.00 o_ 5.5" i s.o" 4,,54 +i +'"_ 3.0" >" 2.0i t.0 i Ntn . _ Tenn. River Valley Samples Pace 3 3M Environmental Laboratory Paoe 214 of 276 Repo_ E02-0443 i IIIIII . _ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY051.D Report Date: 19-Nov-2002 14:49 Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY051.D Lab Smp Id: 0453-38045-3 Inj Date : 12-N0V-2002 16:44 Operator : mla Inst ID: itchy.i Sr_ Info : E02-0443-38045-3; Misc Info SL-3; MeOH Extract; 21 Oct 02; MI._. Comment : Method : \\Etstarget\target\chem\itchy. i\I021112 .b\I021112 .m Meth Date : 13-Nov-2002 09:16 itchy.i Quant Type: ESTD Cal Date : 12-NOV-2002 AIs bottle: 33 Dil Factor: 1.00000 12:14 Cal File: ITCHY026.D Integrator: Falcon Compound Sublist : all. sub Target Version: 4.12 !] .I _._ '?! .! I Oomlx_Jnclm Namii_amm ,=_mlw s 8mm _m_ im= I PPB..q (299} 2 PFH5 (399) 3 ppO,% (413) 4 POSA (49Q_ 5 PP08 (499) _t_NT SZ_ JtA38 m= 299 299 299 399 399 399 413 413 413 495 490 499 499 RT mlil 3.402 3.950 4.309 3.730 3.431 4.039 4.049 3.711 4.300 4.&97 4.508 4.229 3.930 EXp RT mmsmiimB 3.4Z2 3.422 3.422 3.830 3.030 3.030 4.020 4.020 4.020 4.K67 4.067 4.199 4.199 DLT RT i==l_amm -0.020 0.520 0.007 -0.110 -0.399 0._09 0.029 -0.309 0.358 0.030 -0.379 0.030 -0._69 RRSPONS= hi= =,.==m 564505 2069 10856 12125 3434 11470 54999 12405 12568 &5_55 4044 43048S 4504 o_- co_ {ng/mL) siimm=i 10.0353 933.642 0.00434 0.33905 0.13055 0.33490 2.32242 744.930 744.915 _..GS15K 0.22117 9.12623 1354,43 VZm%L (ns/mL) mma=_mu 10.0 934 0.00434 0.339 0.130 0.325 2.33 745 745 _..65 0.2al 9.13 1350 3M EnvironmentalLaboratory Page 215 of 276 Report E02-0443 - _ Tenn River Valley Samples Data File: %%EtstaPl:et%tarCet%che_\/tchu.t%IO21112.b%ITCHY051.9 2,3- _.%t star'l_et\t ar I_et,'_che_\ i tch_. | % 10211_,2. b',,I T_051. D .2- Pae 2 _..0- 0.9" 0.8-" ^ 0,7: .. 0.6" >. 0.15- _ : 1 0.4- i !I 0.2" 0.1" k ",-I-":-,. ) .... i .... _ .... I .... _ .... ) .... i .... i .... ! .... i ....... ) ............ _ .... 0,5 1,0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5,0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9,0 _LPFBS <299> B.5_ 50-.: 45-_ Ion 29900 I _"],oi ". '_i_ ....... 2.8 3.2 3.6 4,0 4.4 2 PFHS 39_)) : Ion ;_9.00 :._ 9.o'_ :'i "o.6"" ", I_ " h II e.o_ >. 7.8 7.6- 74- 7.2" 3.40 3_0 3.80 400 4.20 -: ..... " '" ' C":.l.c , 3M Environmental Laboratory _,_ T)_Rr_ _"tR Report E02-0443 . _ Tenn. River Valley Samples Data File: %_IEtstarEet%ta_tet_v-..he_%itch_j.i%IO21112.b%ITCHYO51oD 3 PFOA (413) : Ion 413,00 o ,_- : )- >-0,90{ :A/\/', 0.70:. , __o 3.60 3.80 4.04) .in 4 FOSA (498) . . . o. . 4,,20 4.40 ,_ ..ei g _. t Ion 498.00 ,. 8.0_ II I- i ,.,, I\ ' ,.o_ I\ ' 'iii! _/ \ / 3.o=.')_ . ) . . , . . . , . . . | . . . 4.40 4.6<) 4.BO e.(x) 5.20 HiP 5 PF05 499) ,. ..o- Ion 499.00 g _. i1 ,".!i fIlI" ., i.o \ ..'! 4.0_ ). 30" o : I"I ,.o4_ _ _,.o- _ 3.80 4.00 4.20 4.40 4.00 Hln ] .% l Page 3 I ;:- .:.; '.A; _ . . c(_.<,/_1,of<_,. 3M EnvironmentalLaboratory Page 217 of 276 ReportE02-0443 . _ Tenn. RiverVailey Samples Data File: \\Etstarget\target\chem\itchy. Report Date: 19-Nov-2002 14:49 i\I021112 .b\ITCHY053 .D Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY053.D Lab Smp Id: 0453-38045-MS(3) Inj Date : 12-NOV-2002 17:06 Operator Smp Info Misc Info Comment : mla : E02-0443-38045-MS(3); : : SL-3; Inst ID: itchy.i MeOH Extract; 21 Oct 02; MLA Method : \\Etstargetktarget\chem\itchy.i\I021112.bkI021112.m Meth Date Cal Date : 13-Nov-2002 : 12-NOV-2002 09:16 itchy.i 12:14 Quant Type: ESTD Cal File: ITCHY026.D AIs bottle: 34 Dil Factor: 1.00000 Integrator: Falcon :. Target Version: 4.12 Compound Sublist: all.sub _ Compound_ mmmmmmmmmlmmmm=mmms=m=nnmm 1 pFJSS |299) 2 PtqIS (399) 3 PI_A (413) 4 pOJSA (498) 5 PP0S (499) QtL%NT BIO MASS mmmm 299 299 299 399 413 413 498 499 499 RT _amu 2.422 3.940 4.289 3.820 4.020 3.691 4.867 4.399 3.920 EXP RT DLT RT RESPONS3 mmimm=mm =mmmmmm= wn==._== 3.422 3.422 3.422 3.830 4.030 4.020 4.057 4.199 4.299 0.O00 0.815 0.567 -0.010 0.000 -0.329 0.000 0.000 -0.279 1B40798 3713 118796 1695558 691396 6715 1092519 12853;9 2917 CONC_TRATI ON- COLUMN ONS FIRAL (ng/mL) =..._m_ (ng/mL) u_mmmum 48.9348 933.S09 2.88083 37.8097 40.375= 745.250 25.9793 29.9181 1354.46 45.9 934 2.88 37.8 40.3 745 25.9 29.9 1350 ? i ,ii ., C--;!!C - 3M EnvironmentalLaboratory Page 218 of 276 Repod E02-0443 I , _ Tenn River Valley Samples Data File: \_EtstarKet\tariet_che_\i_i_j.i\lO2_lZ.b%lTCt_fO53.D 2.9_ 2.e_ 2.7_ 2.6_ 25 i Z.4_ 2.3i 2o2_ 2.1_ 20i _Etst_=et\taret\chem_itch_.i_lO21112.b_ITCHYO53.D Pae 2 it.54_ i 1o2_ 1o_ : o.7_ = o.._ 1.34 t 0,3_ 0.2_ j _$;_.i;6_i;_23_2;_;6_;5_;_;5_;;_5;_;;._;5_._;_;5_8;;_b;_9;_._ 1PF_S(299) 2._ Ion _99_.OO :! 2,1: .: i.o: :I iz_ _ ! i.52 o.3_ .|. , ........ 2oa 32 I __1i ! - 3_ 4,0 4.4 2PF)_ (_) Ion39900 ] 2.72 m ! z.4:. _ 1o5_ 0o9_ 0.3_ 0.6;, IJ _._ 3.40 3.00 3,80 4.00 4.20 .... Hin _" _ ""; _: ,s:_:_ 3M Environmental Laboratory Paoe 219 of?76 Report E02-0443 D_ta Filo: %_Etstm*,ot%t_;et_che_it_d.i%lOZlli2.b_ITowo53.D 3 PFOA (413) ioi-_ i.0_ 0.9-." 0.8- 0,7-.' 0,6" o,6-_ Ion 4:L3. O0 o ,: 0.3..: o.z; ,; 0*oi'4."l-.' L n/ . o , = . .. o-.- 3,_0 3,80 400 Mtn 4 FOSR (49_) J o- - o - 4,20 4.40 i.6: i.4" 1,2.: i.0- Ion 498% 0.4- 0,2-" :. .I J o - a o o o . i 4.40 4,0 4,_0 5,00 15,20 .in E PF0_ (499) Ion 499..00 t '.'! 0,9" t0.o6"-: 04" o., ,J I | o" -. i" 3o1_) 400 4,20 H_n , I__ o o 4,40 4f_ } } . _ Tenn.River Valley Samples Pai:e 3 : .'._':C_,u,'_r:j_;Originai 3M EnvironmentaLl aboratory Paqe 220 of 276 Report E02-0443 . _ Tenn. R_er Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY055.D Report Date: 19-Nov-2002 14:50 Page 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY055.D Lab Smp Id: 0463-38046-1 Inj Date : 12-NOV-2002 17:28 Operator Smp Info Misc Info Comment Method Meth Date Cal Date : mla Inst ID: itchy.i : E02-0443-38046-I; : SL-2; MeOH Extract; 21 Oct 02; MLA : : \\Etstargetitarget\chem\itchy.i\I021112.b\I021112.m : 13-Nov-2002 09:16 itchy.i Quant _"_/pe: ESTD : 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle: Dil Factor: 41 1.00000 Integrator: Falcon Compound Sublist: all.sub 4 Target Version: 4.12 c.o_pounam msmmussmmm=ulmmliimmslmmm 1 pP'BS (299) 2 ppIL5 (3999 3 PFOA (413) FOSA 5 pOS (498) (499) 00ANT SIG NA..q.q _==1 299 259 299 399 399 412 413 490 499 499 RT EXP RT mimm ===mmumE 3.531 3.422 4.01L9 3.422 4.319 3.640 3.422 3.830 3.422 3.830 4.040 3.711 .020 .020 .887 4.2_.9 .867 4.199 3.930 4.199 DLT RT mu_=l== 0.109 0.S67 0.897 0.010 -0.406 0.020 -0.309 0.020 0.020 -0.289 RESPONSB i=_tEmBB 327390 S00E 8043 17353 14192 53375 7259 120467 41723& 11862 CONCBNTRATIONS ON- COLUMN PINAL (ng/mL} m=_=io 9.94256 933.556 933.471 0.45146 0.38350 2.23055 745.219 2.92155 9.04935 1354.25 (ng/mL) =_i=m=i 6.9 934 933 0.51 0.383 2.23 745 2.92 9.05 13_;0 .I I ,.) ..... ) 3M EnvironmentalLaboratow pp_,_?71 _f 97_ Report E02-0443 . _ Tenn. River Valley Samples ]_t.a File: %_JEtstar_et%tav_et%he_%itch_.i\ZOZti12.b\ITCHY055.1) 1.0: \_Etsta-set_tar_et__\ito_. i\IO?-IIi2.b\ITCHYOI5_5, 0.9- 0.8-_ 0.7" 0,6" o o._" >- 0.4" 0,32 0.2" Pae 2 O.i: I_L .... | .... i .... , .... , .... .... , .... P .... i ........ , ................ I .... m.... e .... _ .... o .... 0._ i.O i._ 2.0 2.5 3.0 3.E 4.0 4.5 5.0 5.5 6.0 .5 7.0 7.5 a.o 8.5 9.0 Htn i Pt'IS(299) i Ion 299.00 3.0" i 2,7 ;I ^ 2.i V :! _ =.z" /_ ; s.., 2.a . 3.2 Htn o| .. o.-i 3.6 4.0 4,4 2 FF14S(399) lot, 399 oo 7., _ )_;_CI _,/_,upy o: Ongina) g,8 3.40 360 3.80 4.00 4.20 Htn 3M Environmental Laboratory _,_== o99 _ 9_ ReportE02-0443 Data File_ %_JEtstarget%target_lem%itoh_.i\IO2ili2.b\ITCHYO55oD 3 PFQ_t (4i3) Ion 413.00 0 ; i.10- II _ .=i rl 0.90 i o._ - '_i-.,// 0.70,---%\ (_ _ /.) \_/ ! \\. 3,00 3.80 4.00 4.20 4.40 Hi. 4 F-OS(A49G) Ion 499.00 . i t.4- i _.z" I._, ! i.o" "_ 0.8" 0.6- / 0"4 i_-_._ __, i*, - 4.40 4.60 i *, 4.80 B.O0 . ; _S.20 ' ; i,.i i 8 PFOS (4_3 Ion 499.00 7.0" : ,; _.o_ ..o" i,.o- _" : o ' ,* 3.80 .* *- .* *. 4.00 4.20 MI. D . * 4.40 4.60 _ Tenn. River Valley Samples Pa;e 3 _:2fac/Coopf;O; rigina; 3M EnvironmentalLaboratory Page 223 of 276 Report E02-0443 ._ Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\itchy.i\IO21112.b\ITCHYO57.D Report Date: 19-Nov-2002 14:50 Page 1 3M Environmental Laboratory = _, i J 't ii:t _I Data file : Lab Smp Id: Inj Date : Operator : Smp Info : Misc Info : Comment : \\Etstarget\target\chem\itchy.i\I021112 0463-38046-2 12-NOV-2002 17:50 mla Inst ID: E02-0443-38046-2; SL-2; Me0H Extract; .b\ITCHY057 .D itchy.i 21 Oct 02; MLA Method : \\Etstarget\target\chem\itchy. Meth Date : 13-Nov-2002 09:16 itchy.l Cal Date : 12-NOV-2002 12:14 Als bottle: 42 Dil Factor: 1.00000 i\ I021112. b\I021112, m Quant Type: ESTD Cal File: ITCHY026.D Integrator: Falcon Target Verslon: 4.12 Compound Sublist: all.sub CmP<_u'n'_" ==mnmmmmmmJmmmms_si=mmm=ma I PP136 (29%) 3 PFH -1 (399) ] P];'QA (413) 6 pFO8 C499) FOJIA (491} QC Flag Legend M - Compound response QUANT Big MwAnS.=S 259 299 299 299 399 399 41"1 413 413 499 499 468 nmR=T=s wmEXmP=ssRmTl 3.SII 3.960 4.06% 4.319 3.422 3.432 3.422 3,422 3.840 3.432 3.830 3.830 4.040 3.711 .369 .020 4.020 4.030 ==D=L=Tml=R=T== Rt=ElmSPmOmN=SnE 0.089 0.S3B 0.667 0.097 232749 2G50 5270 7437 0.010 -0.396 18434 20644 0.020 -0.309 0.349 35197 ?(29 12091 CONCBNTRATZONS ON-OOLt_N FINAL =(ln==gg/=m=L) 6.18266 933.62 =; 933.560 933.488 0.47471 0.30=;07 1.20373 745.199 744.948 =(=n=g=/nm=Ll } 6.10 9)4 934 933 0.475 0.306 1.20 745 745 4.229 3.930 4.807 4.199 4.199 4.667 0.030 -0.269 0.020 393650 1297%, 103503 8.49146 1354.23 2..52745 0.49 1350 2.1;3(N) manually integrated. 3M EnvironmentalLaboratory Page 224 of 276 Report E02-0443 Tenn. River Valley Samples _ata Filet \_Etstarget_t_Eet%ehem%itch_J+|%IOZlllZob\ITCHY057.]) %_JEtstarcet\tar Ee t\che_,i to_ I.i\1021112 .b\l TCHYOS7. D ii- ! 1.0" : 0.9- 0.8: 0.7- i 0.6- Pae 2 i 0.3; '! o.z! 0._: J__ Ht_ : i PFBS (299) i t Ion 299.00 ; 2.z-.: _'i + z.o" 1.8-'. " "_i ^ i.6: I'_ : '+-. :- 2_o..oe."-4_ i . !,.++ 0,6_ 0.4" 0.2! "2'.9" "3;i" _:i" Hin r;, +'.o" +:_ 2 PFHS (399) Ion 399.00 _.:i! ,....,.'- " 6,6:- '_ _ .. : Q'l?(/,_/>_/__ " 5oG t . . . I - . i . + *1. 3,40 3,GO 3.80 4.00 Hip . . i. . 4+_:_ 3M Environmental Laboratory Page 225 of 276 Report E02-0443 . _ Tenn.River Valley Samples Data File: %_JEtstarKet\t_Pcet_he_\itohs, i_IOZili2.bNtTCHYO57I] 3 PFOR (4i3) Ion 4i3 O0 o o.$6-_ II '_-= /L o.aa" IL o..8-o-_ _. tt l I 0.76- '_ t I 0._ ix / _ o,_e-'.1. \ / \ o.64-..J,,,s\ / x.,. o._o -| _ , i , 3.GO 3.80 4.00 4.2 H;n ; ": #,, I_ /\ I\ ! \, * 4.40 4 F'OSA (498) Ion 498.00 p. I.G i : " _.o: ,1..24.. _ / >" 0.6" 4.40 4.60 4.ao 5.00 Ei.20 H:An i _ PFOS (499) .i Ion 499.00 o G,,5.; m "-_ 5.5" i _.i ! 4.5.; ii i 4"-."--; >. 2.5_ 2.oi _, i,O_ t_ l o.S_L J . , , , 3.80 4.00 4,20 4.40 4.60 Pa;e 3 "_ CopoyrOriQinaj o 3M Environmental Laboratory oo_ _ ^, _-:,_ Report E02-0443 . .. Tenn. RiverValley Samples Data File: \\Etstarget\target\chem\itchy.i\Z021112.b\ZTCHY059.D Report Date: 19-Nov-2002 14:50 PaHe 1 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I021112 .b\ITCHY059 .D Lab Smp Id: Inj Date : Operator : Smp Info : Misc Info Comment : 0463-38046-3 12-NOV-2002 18312 mla E02-0443-38046-3; SL-2; MeOH Inst ID: itchy.i Extract; 21 Oct 02; MLA Method Meth Date Cal Date : \\Etstarget\targetkchem\itchy. : 13-Nov-2002 09:16 itchy.l : 12-NOV-2002 12:14 Als bottle: 43 Dil Factor: 1.00000 i\I021112 .b\I021112 .m Quant Type: ESTD Cal File: ITCHY026.D Integrator: Falcon i Target Version : 4.12 Compound Sublist : all. sub _ Co_pounds =._lim =,._jmnnniB mm_amsum_ =,== I PFBS {399) 2 Plqi.q (399) : i 3 ppOA (413) i :_i 4 POSA (496) i 5 1_08 (499) <,_ i QUiT gig MASS =Rim 299 299 299 399 399 413 413 413 49 499 499 RT nllm 3.S41 4.090 4.319 3.850 3.432 4.040 3.711 4.369 RXp RT DLT RT ma=nmi .,='n .n===.=l 3.422 0.119 3.422 3.422 0.660 0.897 3.030 0.020 3.830 -0.398 4.020 4.030 0.020 -0.305 4.030 0.349 4.807 4.867 4.239 4._99 3.9304.199-0.269 0.030 0.030 RESPONSE Ism a.l_ 420079 6904 11583 29494 17014 40917 8900 11304 133292 47090? 14760 CONC_TIONS ON-COLUNN PINAL (ng/mL) mSRunRm 11.6624 933.503 933.369 0.62694 0.44417 1.52653 749.145 744.964 (ng/mL) I_=tliu 11.7 934 933 0.626 0.444 1.$3 745 745 3.21670 10.s027 1354.19 3.22 10.S 3360 v_ ! 3M EnvironmentalLaboratory Paoe 227 of 276 Report E02-0443 . _ Tenn. River Valley Samples Report E02-0443 Tenn. River Valley Samples _t.a Filet ",%I_Esk=_-_te.\t.ar Cet.'._che_(.\r.r.,r_,i %107-t.112b, %I_9, D 3 PFOR(4'13) , 1o30= lore 4_.3.00 1.20i _._i ,, _.to-: :I II tl ., _o.,_i A 11 h _-o.,o_...,//J \ ]_ 3.fPO 3.80 4.00 4.20 4.40 tl_n 4 FOSR(49g) Ion 498.00 r*,. 1.4" l.s-' \ /\ | i e . , i - 4.40 4.60 4.80 5.00 5.:)0 HSr,_ 5 PF(3_ (4_) Ion 49c_.00 :i 4._ 3.0i ,_ 2,0-" __ ,_ .:: i Pal_e3 ' .: - .,.l' , 3M Environmental Laboratory i Page 229 of 276 i ReportE02-0443 . _ Tenn. RiverValley Samples ATTACHMENT D: SAMPLE PREP SHEETS, TEST SUBSTANCE, AND TEST SYSTEM INFORMATION 3M EnvironmentaLl aboratory Page 230 of 276 Report E02-0443 . _ Tenn. River Valley Samples ._ Tennessee River Valley Samples Lab r,_ Sample Location 1, Large Mouth _t 3M Environmental Laboratory Paoe 231 of 276 ReportE02-0443 Tenn. RiverValley Samples LabRequest: I cJ) Tennessee River Valley Samples SampleLocation1, Catfish SL4c..1_ _ SL-1. C-2-2 _ SL-1. C-2-3 -_ SL-1. C-2-MS "_ _, _ _,S "_- ,'_ -'_-I s,-,.c._-_.,-,_- < _ _ _ _ _ _ _- _ _ _, s,.,._-, :,o_._:,_.. ,. _. . ... ,,._ SL-1, C-4-MS _ .. |1 _,J I_J s,-,.c_, _,0_I " "_; ._ _ _ s_.,.c-_-_ _ r_ ;:: .'_ '_ _ ,., ,_ _ _j! SL-1. C-8-3 s,..,,c..,.,-s- . "I SL-1, WB-1 _ / "] <-_ _ # SL4,Se4 ......... _; SL4,SS-Z "-" y ..... i " !' - ..... 61=_ co,,,,=_,,o,,o._c._,z._.=,__.,/,_,,,_'' co,.,,.k.,.,,C)_ q' alance ,D .__ Tuloetype/_IzeP_/'//tt_ ) _0_ L Zq_l StartT/D/I.L_._l.___(_c Water ID _; _; -_ "_'(_t,(__ Col 10 T/D/I _.._I11rlO,_11_. t _: t"c" _ "_ i ao,.,.,..=.,_..,_,=,,,. a_ ,_.d3_ Col 7 Spiking Standard ID # ___..____ "1 ApproxlmaleConc. ( r_,_t Amou,tadded__L_. TID/IJ[I:IL)_,Hpw% _J? I t(_" /0")" _I_ CO i _j: ThJ(}-_qO,_ el: _,O,t-M(,/_z/o_-_,_(: 3M Enml'onmenlillLIItx_llory 3M EnvironmentalLaboratory co,,-,-,,__,,._. ._ L,.L_.C.,..__ Col 13 T/O/I _._ (_10 .__ I'P('- C0, t4 T/D/I IO'.J_J..L/_._,___...Cw I-(,- MeOHID: TN.A +_'_'_0 V,j/d)vO-,_'_'/-_/p,,r_.,,) 0 L,7', ,.,-H/-z_f.4:o,_. t", .,.4 -n_-1;/_ - ,..,,4._,_,o.,,#,_ O,,I.l"-.t_" :=v,._,l_) _,,.(v _p./,'_J _,. _lep 7" .."'/_ "/IP,'r 6 ') Page 232 of 276 Report E02-0443 . .. Tenn. RiverValley Samples LabRequest_:.- _V,_ Tennessee River Valley Samples Sample Location 2- Large Mouth & Location3-Small Mouth 3M EnvironmentalLaboratory Paae 233 of 276 ReportE02-0443 I . .. Tenn.River Valley Samples 3M EnvironmentalLaboratow P_n_ ?_ _f _'_ ReportE02-0443 II . _ Tenn.RiverValleySamples LVo Request t11.)=_tl)J _ Tennessee River Valley Samples Sample Location 3, Large Mouth 3M Environmental Laboratory Page 235 of 276 Report E02-0443 . _ Tenn. River Valley Samples _M Environmental Laboratory Paoe 236 of 276 ReporEt 02-0443 . _ Tenn.RiverValleySamples ReportE02-0443 Tenn. RiverValley Samples 3M EnvironmentalLaboratory Page 238 of 276 Report E02-0443 i II .... Tenn. River Valley Samples Lab Request:_ _/_-J'l rt/_ Tennessee River Valley Samples Extracted Curve Information 1 2 3 4 5 II 1 I 10 I 11| ( , 12 '13 14 i IS "" _'" ' "---- _rt P,k , )y, l, ,. L_L'_ LIt_'_I t(,_)L/V 9_,.,( I/ / ,_ (,/ l/ U" L,,/ / V V" L.,/ .e,'_(t;_l;_,,_41)l)tt/]t "-,.... ,_._ .., WaterlO _l;/_"_ T(./ P(_; co,. ".o.0_'5_; ;X ,:.J.__JE. __s_..,_,_'-,_T.___ : ! _",_\ ... .;_ -_ ColIO T/Dn,,I$_() _l /_,_..._/(_.J/l t_- I,._ c.,=,_.,o: T4_ i RCF/_Ru0OUt: Minute= ,_.0 c' Temp'C/-b'o_'f'C_zJ Cole t;_.ltoo :t1 IJ"_l _'I1_ Col7 SplklngStandardlO#,_0)'_-_ _# t _,) O,tJ .015 ..#_---_x"/_ .l,_ Col 12Trol_l,. t,,w, WaterlD_//_;/);-0 TO(p)o.') Coi13 TIDII I ._)_'') _1>1.7._.1_j')//l_ 3M Emeor_, L,iC_x'atory 3M Environmental Laboratory Page I o_ Page 239 of 276 ReportE02-0443 . _ Tenn. RiverValley Samples Non GLP SPEColumns Extraction Worksheet Prep Date: 6/20/2002 Analysts initials: OK Method Revision: _ Study Number: E02-0443 _:) #o E-TS,..,'/_,J u,.D. ,",_-//_,, ='_ Sample Number or description..... Volume ot sample filtered water blank 40 ml Type of column used i lg, 6ml,C18 lot2057e2 Amount and spike mix used i NA Elution solvent andl volume MeOHTN-A-6116 2mI Comments ii |l E02-0443-38025 40 ml lg, 6ml,c18 lot205762 NA MeOHTN-A-6116 2ml E02-0443-38026 40 ml 1g,6ml,C16 Jot2057B2 hA MeOHTN-A-6116 2ml E02.-0443-38027 40 ml lg, 6ml,c18 lot205762 NA MeOHTN-A-6116 2ml E02-0443-38028 E02-0443-38029 40 ml 40 ml lg, 6ml,C16 lot2057B2 lg, 6ml,C18 tot2057B2 NA MeOHTN-A-6116 2ml NA MeOHTN-A-6116 2ml E02-0443-38030 40 ml lg, 6ml,C18 lot2057B2 NA MeOHTN-A-6116 2ml lg, 6ml,C18 NA MeOHTN-A-6116 " '] E02-0443-38032 40 ml tot2057B2 2ml ! E02-0443-38033 40 ml lg, 6ml,C18 lot2057B2 NA MeOHTN-.A6- 116 2ml E02-0443-38034 40 ml lg, 6ml,C16 lot2057B2 NA MeOHTN-A-6116 2mr ;! E02-0443-38035 40 ml lg, 6ml,C18 lot205762 NA MeOHTN-.A-6116 2ml E02-0443-38036 E02-0443-38037 E02-0443-38038 40 ml 40 ml 40 ml E02-0443-38039 . 40 ml ; E02-0443-38040 40 ml ', E02-0443-38041, 40 ml , E02-0443-38042 40 ml _, E02-0443-38043 40 ml lg, 6ml,C18 lot2067132 lg,6rotC, lS tot2057B2 lg, 6ml,C18 lot2o57B2 lg, 6ml,C18 tot205762 lg, 6ml,C18 lot2067132 lg, 6ml,C18 lot20576Z lg, 6ml,C18 lot2057B2 lgl,ot62m0l,57C1B82 NA MeOHTN-A-6116 2ml NA MeOHTN-A-6116 2ml NA MeOHTIC-A6-116 2ml NA MeOHTN-A-6116 2ml NA MeOHTN.-A6-116 2ml NA MeOHTN-Ao6116 . 2ml NA MeOHTN-A-6116 2ml IdA MeOH T2Nm-A-l 6116 ' E02-0443-38047 40 ml lg: 6ml, C18 lot205762 NA MeOH TN-A- 6116 2ml // Extraction Steps initialWhen/if done): C,d,.;condition column with MeOH; c_PL'_w_.a..s, h with milliq; _ t_" rifler sample; t :..K_vacuum dry the column; c.P_, elute column with solvent; _t:---,transfer extract into an autovial .i , Additionaclomments: (c "/ O(E" -e.'-(__)__,,L_c:__P'c:_ _ =_'L' E'L.P ! Fr.xC_op'oJ:0_,g'_n_' 3M EnvironmentatLaboratory p_t,_ _,_n,_(_7_ ReportE02-0443 . _ Tenn. RiverValley Samples Non GLP SPEColumns Extraction Worksheet Prep Date: 7/17/2002 Analysts initials: OK iml Sample Number or description Volume of sample filtered water blank 40 ml E02-0443-38026 40 ml E02-0443-38027 40 ml !E02-0443-38028 40 ml E02-0443-38030 40 ml Type of column used lg, (_mlC, 18 rot2O57B2 _lg6, mr,C18 Jot2057=9, 2 tg, 6ml,C18 1or2057B2 lg, 6ml,C18 tot2057B2 llgo,t_20l,57cB128 Method Revision: E__3._,,_ E.t Study Number:. E02-0443 Amount and spike mix used NA NA NA NA .... _ Elution solvent an( volume MeOHTN-A-J_ '' 2ml MeOHTN-A-_H'6 2ml MeOHTN-A2ml MeOHTN-A-,_H15 2ml ' _oHT2m_,l_-'6,U_, Comments ., ,.... I ,I -.... , -..... "_// /, ; \ Extraction Steps (initial when/if done): ndition column with MeOH; _.._...wash with milliq; __.._filter sample; cuum dry the column; _j2_alute columnwith solvent; O_L.,..,..,..,..__treaxntrsafecrt intoan autovial Additional comments: _,lCt CoP_C_"_,ii_ 3M EnvironmentalLaboratory p=,, _a_ _* _ Report E02-0443 - - Tenn. River Valley Samples ReportE02-0443 Tenn. RiverValley Samples 3M EnvironmentaLl aboratory Page 243 of 276 ReportE02-0443 Tenn.River Valley Samples 3M EnvironmentaLl aboratory Page 244 of 276 Report E02-0443 . _ Tenn. RiverValley Samples ReportE02-0443 . _ Tenn.RiverValley Samples Oate_: I C'_t _ Analyst: /_' ( ._- SINGLE COMPONENT PREPARATION LOG BooN_o.02o_o PageNo. 34 StockNumber. _._ '_.__'_."_ " _ "J_ I ! Weightor Volume :. usod: / _ 0 u L. ] ,i Concentrationor Purity: )//_ t_ ,_?_ CorrecteWdeight: "--" i '! FinalVolume: _ Lh _v/i[.. BalanIDc:e .,4/_ OtherCorrection Factors: Solventand TN-A Number./_ _ _/m :7 L't,,_,/- /p [_I,II,.._ To<I'/_._) FinalConcentration: ) _'_/9_ StorageLocation: . -__..L_,EZ:/_.* ExpirationDate: c_ -'_ _<4 u/ _,l i 'i Exzt Co_ of Odglna] L?" ,:./i. ," si_t1,,9,_,<.c.c,."-L,_(.,_d,._t,..'i:._,D=, Reviewedby: (J-- . /(/( / d'_._ 3M EnvironmentaLl aboratory Page 246 of 276 ReportE02-0443 . _ Tenn. River ValJeySamples ._ MULTI-COMPONENPTREPARATIONLOG BookNo, 02 002 i oesc._o_n'-'i,_,h 3p;_e / i DatePrepared: (_ t_'f O _)--- PrepareBdy: CJ_t.,tC,. i storagLeo=Uo.: o_Ct ExpirationDate: | I / _ :'_) C_"J-J i StandardID # ' 02 002-33 i= ii J PageNo, 33 So,veHn_t:C_ 3M Trace#: TN-A- (Dll(D I ComponenSt tandard Corrected FinalConcentration Conc.or Expiration Weightor Weight Description ID# Purity Date Volume BalanceID 3N- v,olo3 , <tc__ _ _"-- t_.l ;_l_'i .._.--_ .... FinalVolume EcaCct0p0yf0rtlllnal inlllal D_ -:'L. L 3M Environmental Laboratory ii _t,y_ L Concentratioonf the mix i ,,,,,, Signature, Date Page 247 of 276 Repod E02-0443 III . _ Tenn. RNer Valley Samples ii Ii II i II I .,J t i ..+ . 'l I i ..+ Date:_ _a / I_ / O'L SINGLE COMPONENT PREPARATION LOG BookNo. 02 022 PageNo. 77 I(J_ _t',<: t-I s_ X.mberC_ _vr_+n WeiglltorVolume ConcenmUoonr PUd_:_ . ^ +,pp +.', j+,e. ,+ !+I" -+.Q_,+ j,e?- vl ., (e I' '/ _1; u,J i +,i___*'- n '-+- Sok_ntandTN-A t Ii i/ .,. / i .11 3M Environmental Laboratory _grmgim, DaW Page 248 of 276 ]1 ReportE02-0443 ._ Tenn. RiverValley Samples II J SINGLE COMPONENT PREPARATION LOG Data: fl _,"O"/ _ BookNo. 02040 _,_.. ,H/_ _,o,_o. 80 Ii all L _2 j tl ;a _ a 'i i 2:.p .; I - TA,'-A- f/ 7- Weightor Volume - II,repOJ Corcentmtioonr qq.re, % _,_: OtherCorrection ,,,V'A Cor.,=,Wn ,_ht: A/A so_t a,.,.,T,.N=.A__.,/h.(_ 7,0( P/_,s _-,=,_o,u,,.,._: L _-.,Co.o..,_.,_l ..: _=_.,-a=,..: "_FIr f'c,o _._.,.: _9_/v,_,(,9) -. i . ".L .2t_ _ i / 3M EnvironmentalLaboratory Pane 249 of 276 Report E02-0443 . _ Tenn. RiverValley Samples .,. II m g SINGLE COMPONENT PREPARATION LOG Date: J/O" O,,_ a Analyst: _VJ BookNo. 02 001 PageNo. 17 i Oe_on: 73r"ft 5 m stocNkumber. _# - O _ a WeightorVoUlsuemde: _ 'C")(_O_ " o I! Concentratioonr _ I i a == StorageLocation: (_t (_ J_O_ BalanceID: c_ JL.] OtherCorrection Solvenat ndTN-A ExpimUoDnata: _.|O,E') _ a 3_I EnvironmentalLaboratory p_t_ 2_0 of 276 ReportE02-0443 , _ Tenn. River Valley Samples I ml i u ii SINGLE COMPONENT PREPARATION LOG Date: /-/O,O_ m Analyst:. OF-, SeekNo, 02001 PaoNeo. 1_ Description: _ _/i_ al 11 StockNumber:. ,E_ 0o_.(_ we.,oUsredv: oL,O.o/m/7.7 t Concentratoiron t Purity: , _Jto_ , .; CI I CorrectedWeight: ,_,1A BalanceID: C:_IL_ OtherCorrection Factors: , Number:. ,= EcCtCopVo! 0rigir_! S_gnztu/m-.- " I z_ate al o 3M EnvironmentalLaboratory Page 251 of 276 Report E02-0443 . _ Tenn. River Valley Samples I I II III I I SINGLE COMPONENT PREPARATION LOG Date: C_ F,p/') (_2 "= BookNo. 02 001 PageNo. 84 I I WeightorVolume 6_ :Ii - 4 Concen_Uonor --'- Purity: ' II i ; _ a ! , ql " I '--"-CorrectedWelght: FinalVolume: "_ _h/L StorageLocation: _ d f/_ ExactCopyof 0dginal " I I OtherCo_e_n Fa_om: SowentandTN-A . / _ ..."AI -Tit_ /I r'A/;-/ Number.iTry,{.ln_-I izv z_- ,X/x( t F ,/_"_'//,4, o< FinalConcentration: <=_3__) ('_l_rn_ ExpiratioDnate: _ g _b _ 3M EnvironmentalLaboratory Page 252 of 276 Report E02-0443 . _ Tenn.River Valley Samples i I Ill II SINGLE COMPONENT PREPARATION LOG Date: _) _ f_o _ (_ d ,_a_t: /_," BookNo. 02 001 _,No. 85 " _..<.p,__.C: -lq3/pfoA 4 a Used: We_htorVolu_ @. J_"7 7_/_ BalanceID: fi_ il i i ill FinalVolume: ;:::;S> _L FlnalConcentraiton: .,_/7_/_Fl.,w Ill .; II Ii t ExacCt opyof Original Si_'_a_, ) Da_._l 3M EnvironmentaLl aboratory Page 253 of 276 Report E02-0443 . _ Tenn.River Valley Samples i II ,.. li J am ai SINGLE COMPONENT PREPARATION LOG al o-: __,/_::::)., [ ^=_,,t /u/ IA _,,o. 020=2 P,_,,o. II De=_on:PT:B_;//.- "--tOSgZ,ot'=) (c_l:._so, g) al = Weightor Volume ,, --: _.s__s_ i ,_,:, q. 7.3% i ; ,, _ w._ & _fq_j t Jlld " ill I. ,,> FlnlllVolunilr- _ 5/'p ) ,.,.--, :Y.v'sg/,,. I / ,n.,o: q/el o. C--.n Factors: Solvenat ndTN-A ,--. ,,,,_1.O/-Z7.N -.4--(,_I/I,S FinalCo, rlcenlridloin" "' I _ 7_:]el_ Ugg L .,.o.,>.: :_ A'<,_,,, s_=.,,// b/ - o,to" / 3M EnvironmentalLaboratory Page 254 of 276 Report E02-0443 . _ Tenn. River Valley Samples I I == t" a all i iii I oa=: _(?3-_n,_ A_,_,t:.. C_M. SINGLE COMPONENT Oz- PREPARATION LOG BOOkN0o2.022 Page No. 79 I= III ! 1" m g ', ,, == -{ Stock Number:. (_ - _'_ Weightor Volume Used:.... _0(__. ,IL,,tL- Concentr_on or ___ CorrectedWeight: _ BalancelD: _/Pt Other Correction Solventand TN-A Number:-_J'_e0_ , 'TJ_- 4_-=._ 0 '.1 M Final Volume: I 0 _ b Fllr'l_Coctce.tratJort:_ } pp UI " +, .! StorageLocatton:, , _L ExpiratlonDate: _l/o_/-_/ _-- Sigrmtum, - v - Date a 3M Environmental Laboratory Page 255 of 276 Report E02-0443 . _ Tenn. River Valley Samples I'Cl_"# Substancetrade name or reference#: TCR43 TCR Receipt & General Information ' TCR Substance# SE036 Substance/chemicanl ame: Lot/batch#: Locationof synthesis, fabdcation,or derivation records: Perfluorohexanesulfonate Primary std Receivedfrom: George Moore Date Received: 09/0311999 Amountreceived(wt. orvol): 154 g, 277.38g gross wt. MolecularFormula: Condition: Expirationdate: CSFI3SO3-K+ white powder 10/18/2008 Number/sizeof containers: Shipper: MSDS (y/n) 11150mL glass container Couder Y () N Purity: $6.6% LAC 01117/01 3M # Enteredby (Initials) LAC Std Location/Storage F19, Frozen Amountof Retain 0.3610 g NB 120067-69 Date _:ntered 09/03/1999 ..... Initials initials Recordsreceived: CheckedBy ' Date' Date 10/1911999 MSDS, NMR Characterization Request#59085 Intadm final report from Centre and Certificate of Analysis. LAC 04/20/0t Date Checkedby (initial/Date) Checked by (Initial/Date) Comments initials' Date ' Checked By Date Standard has been moved to Freezer 19 in morn 347 KJD 06/06100 Sent to Centre Analytical for Certificate of Analysis _natysls on 07106/00 LAC 07/31100 Standard was storedat room temperature prior to ; 06/06/00. LAC 12/19/00 I Shipping Codes: 41-2600-g45g-8. LAG 00/14/01 ?I, : Original label - 0/4/99 RWW-11/2/01 ! Shipping comments: NOT REGULATED,3M shipping ID 41-2700-4547-3. LAC 01110/02 ', Attachments N se036msds.pdf N se036nmrreq59085.pd E00-1878-COA-SI=036-PFHS-F1 t (_ ArchivedlSubstanca NOt Available ! 3M Environmental Laboratory Page 256 of 276 Report E02-0443 . _. Tenn. River Valley SamDles I'CR # Substancetrade name or reference#: Substance/chemicalname: Lot/batch#: Locationof synthesis, Pabdcationo,r derivation records: MolecularFormula: Condition: Expirationdate: TCR-29 PFOSA TCR Receipt & General Information el TCR Substance# Perfluorooctane=ulfonyl amide or Pe_uorooctaneaulfonamide AC KJD 7124100 L-15709 Building 236 Receivedfrom: R. Buckanin Date Received: 04/2011999 Amountreceived(wL orvol): 124.98g gross wL CSF17SO2NH2 Number/sizeofcontainers: light yellowwaxy solid MCH 07/22/99Shipper: I0131/2006 MSDS (y/n) 11100mLgtass container Road Runner Y (. _ N Pudly: TBD, KJD 05/05/00 Recordsreceived: MSDS, summary page of FID analysis #57915 3M #Enteredby (initials) NA Date Entered i : LAC i Std Location/Storage Initials i ':?1 AmFo1u9n, FtorfoRzeentain I 0.2233(] Initials CheckedBy Date Date 10118/1999 Date CheWed by (Initial/Date) Checkedby (Initial/Data) 30mmenLs . " Enitials | 3ron weight difference due to removalof parafllm LAG )4/28/99 _itandardhas been moved to Freezer 19 In room 347 _,JD06/06/00 Standardwas stored at room temperature priorto )6/06100. LAC 12/19100 rim explraUon data was assignedbased on hydrolysis Date Checked By Date 'i sthuodwyeEdLt-h1i1s3c2oemnpdopuhnodttoolybseissstatubdley,WL2A7C8310w/h31ic/0h1 : Ddglnal label dated 3/18/97 - RWW 10/25/01 :._ Shipping Comments: NOT REGULATED,shipping code 'i LB4000-t570-9, L-15709. LAC 01108/02 ,; Attachments sd029msds.pd sd029fid57915.p i (,:,'_ArchivedlSubstancNe ot Available! 3M Environmental Laboratory Page 257 of 276 Report E02-0443 Tenn. River Valley Samples TCR Receipt & General Information rCR # TCRo123 TCR Substance# TCR_ " Substancetrade name or reference#: PFOA (POAA) Substance/cbemicelname: FC-143 Ammonium Perfluorooctanoate (Primary Std) Receivedfrom: N/A Lot/batch#:. 332 Date Received: 02/02/2000 Locationof synthesis, 3M fabricetion,or derivation records: Amountreceived(wt.or vol): 278.20 g gross wt. MolecularFormula: CTFI5COO-NH4+ Number/sizeofcontainers: 11-200 mL glass bottle Condition: Expirationdata: White powder KJD-2/2/00 10131/2006 Shipper:. MSDS (y/n) Unknown Y( )N Pudty: 3M # 95.0% LAC 01117101 NIA Records received: MSDS Interim final report from Centre and Certificate of Analysis. LAC 04/26/01 Enteredby (Initials) KJD Date Entered Checked By Date Std Location/Storage Initials Date Checkedby (initial/Date) _t F19, Frozen Amount of Retain Initials Date Checkedby (initial/Date) 0.2737 g 02/17/2000 Comments _Vasoriginally TN-A-2143, KJD 2/21100 Standardhas been moved to Freezer 19 in room 347 KID 6/6/00 standard was weighed on 9/28/00. Standard was storedfrozen at -20C+1-t0C until shipment on 10/03/00.LAC 10/I)3/00 Shipping Codes: 98-0211-0891-91FC-S090-0192-0(<3g0 on dry ice) LAC 06/14101 Standardstored at room temperaturepflor to 6/6/00 LAC-12/26100 Label - recorded.10/98 RWW.1116/01 initials Date Checked By Date Shipping comments: REGULATED-TOXiC Dangerous : goods in excepted quantity of Class 6, UN2811.3M Shipping ID: 98-0211-7394-7,(4 lb. carton) fully regulated. LAC 01106/02 Attachments N tcr99030-30msds.pdf I :., E00-1763--COA-99030--30-PFOA-R 3M Environmental Laboratory Page 258 of 276 i Report E02-0443 . .. Tenn. River Valley Samples TCR # Substancetrade name or reference#: Substance/chemicalname: Lot/batch#: TCR-129 PFQS TCR Receipt & General Information TCR Substance# , FC-95 Receivedfrom: Potassium perfluorooctaneeulfonate AC KJD 7/24/00 215 Date Received: TCR-_3'_,_ N/A 02/02/2000 Locationof synthesis, NIA fabrication,or derivation records: Amountreceived(wt. or vol): 40.144t g gross wt. MolecularFomlula: Condition: Expirationdate: CSFI7SO3-K+ white powder 12/01/20t0 Number/sizeof containers: Shipper. MSDS (y/n) 1160ml nalgene bottle N/A Y I_) N _urity: TBD, KID 6/5/Q0 Recordsreceived: MSDS 3M #Enteredby (Initials) N/A Data Entered =, , CheckedBy ' KJD Date Std Lor_.aUon/St0rage Initials i F19, Frozen Date Checkedby (Initial/Date) !;:_ Amountof Retain Initials Date Checked by (Initial/Date) 0.1867 g 02/17/2000 Comments H Initials Date Checked By Date Nas originally TN-A-2144, KJD 2/21/00 Standard has been moved to Freezer 19 in morn 347 KJD 6/6/00 Shipping Codes: FC-S000-0185-6(<30g on dry Ice) LAC : )6/14/01 ; Standard was stored at room tampemtum prior to 6/6/00 i LAC 12/26/00 Received 5/96 RWW 11/6/01 ,,; Shipping Comments: Dangerousgoods In excepted . quantity of Class 6, UN2811. : REGULATED-TOXIC 98-0211-0888-5(>30 g (t oz :-'_ sample)) Not on dry Ice. LAC01108/02 :i Attachments ..I I tcr99030-36msds.pdf 3M Environmental Laboratory Page 259 of 276 Report E02-0443 . _ Tenn. River Valley Samples TCR # Substancetrade name or reference#: Substance/chemicalname: Lot/batch#: TCR_ PFBS TCR Receipt & General Information TCR Substance# Potassium perfluorobutane sulfonate 2 Received from: Date Received: TCR-00()17-071 Wildlife 06/30/2000 Locationof synthesis, fabdcation,or derivation records: Wildlife Amountreceived(wt.or vol): -100 g, 121.5285 g gross wt. Molecular Formula: C4FgSO3-K+ Number/siZeof containers- 17-100 mL plastic container Condition: good/fluffy white crystals Shipper:. unknown Expirationdate: I purity: 01117/2007 97.3% LAC 04/26/01 MSDS (y/n) Recordsreceived: Y ( )N MSDS Intedm final report from Centre and Certificate of Analysis. LAC 04/26/01 ' 3M # L-7038 LAD 01103/0t i Entered by (Initials) Date Entered CheckedBy Date KJD Std Location/Storage initials Date Checkedby (Initial/Date) _I Freezer F-19, frozen | , i || i Amountof Retain Initials Dale Checkedby (initial/Date) 0.2826 g 06/3012000 Comments Initials Date Checked By Date Wildlife International Number 5292 KJD 6/36/00 Standard I= being stored in Freezer F-19at -20C KJD 7/17/00 Formula added on 07/24/00 by KJD Sent to Centre Analytical for Certificate of Analysis Analysis on 07/05/00 LAC 07/31/00 I; By F-11926 process LAC 01/03101 ' Shipping comments: NOT REGULATED, (based on :, shipping code of LB-1000-07ti3-8). LAC 01110/02 _i_ Attachments tcr00017-71msds.ptcdrf00017-711otinfo. E00-1877-COA-00017-71-PFBS-R ;_Ci"ArchiwdiSubsiaNnoctA'evailai)_J]_ 3M Environment_l Laboratory mmm_,?_C_mf _'fF, Report E02-0443 Tenn. RiverValley Samples ReportE02-0443 . _ Tenn. River Valley Samples 3M EnvironmentalLaboratory Paae 262 of 276 Report E02-0443 Tenn. RiverValley Samples 3M EnvironmentalLaboratory Page 263 of 276 Report E02-0443 Tenn. River Valley Samples 3M Environmental Laboratory Page 264 of 276 I ReportE02-0443 _ Tenn. RiverValley Samples 3M EnvironmentalLaboratory Page 265 of 276 Report E02-0443 . .. Tenn. River Valley Samples ReportE02-0443 Tenn. River Valley Samples 3M EnvironmentalLaboratory Paqe 267 of 276 Report E02-0443 Tenn. RiverValley Samples 3M Environmental Laboratory Page 268 of 276 Report E02-0443 ]1 . ._ Tenn. River Valley Samples 3M Environmental Laboratory Page 269 of 276 ReportE02-0443 ATTACHMENTE: NOTESTO FILE . _ Tenn. River Valley Samples 3M Environmental Laboratory Page 270 of 276 ReporEt 02-0443 Tenn.RiverValleySamples 3M ENVIRONMENTAL LABORATORY i i Noteto File i i i Project or Study Number: E02-0443 LIMS Number: NA Affected Data: D020626Extracted, D020628, D020629, and D020702 (Fish Tissue) mmn 1. The following samples were mislabeled in their respective sequences. They were all labeled as "-1-I" when they should have been labeled as "-1-2". The list is as follows: D020626Extracted: DUDE0055, D020628:DUDE0056 and DUDE0075, D020629:DUDE0063 and DUDE0096, and D020702: DUDE0062. 2. All of the fish tissue sample preparation was done at the same time; therefore, Water Blanks (WB) and Solvent Blanks (SB) were done with each Sample Location, not with each different type of fish from each location. This was done since the WBs and SBs are for examining the sample preparation process and are independent of the species of fish being analyzed. II_e WBs and SBs were analyzed with the Catfish samples. For this reason, there are not any WB or SB data contained within the Large Mouth or Small Mouth analytical sequences. 3. The fish tissue samples were analyzed in triplicate. Each fish tissue parent sample was first weighed out into a container (Column 2), had water added (Column 3), and then homogenized (Column 4) before it was separated into triplicates. The weight are recorded in the %1" rows of the Fish Tissue prep sheets. It is not until Column 6 that the triplicates are generated from the homogenate (MSs are also generated at this time). The samples that were labeled with "-MS" were spiked with the spike solution in Column 7. 4. The fish tissue that was used in the extracted fish curves was from the fish tissue sample with the lowest amount of endogenous analyte concentration. This was determined during a preliminary range-finding experiment. 5. The extracted fish tissue standard curves had a 0 ppb curve point. This point was part of the calibration curve and was "Enabled" in the quantitation software, but it was not calculated as part of the curve. 6. The 10 ng/mL standard curve point in the Extracted Large Mouth Standard Curve had 21% and 22% deviations, exceeding the criteria by 1%and 2%. These points were not excluded from the curves and their inclusion had no negative effect on the data quality due to the point being surrounded by at least two passing calibration points on both sides. i I l! ! O 3M EnvironmentLaal boratory Page271of 276 Report E02-0443 o_ Tenn. River Valley Samples 3M ENVIRONMENTALLABORATORY I Note to File I IIII I Project or Study Number: E02-0443 LIMS Number: NA Affected Data: I021112/River Sediments I I I I 1. Lab Control Samples(LCS) were performedforthe River Sediments. However, the informationwas not used becausethe data suggestedit was impossibleto recoverspikedanalytesfromacidifiedwaterwhen riversediment was not present. 2. The injectionfiles fromthe sequenceI021112 thatare afterfile Itchy062are not partof the reportableanalyses. These sampleswere methoddevelopmentonly. 3M EnvironmentaLl aboratory Page_)_.of .__. Page 272 of 276 ReporEt 02-0443 Tenn.RiverV=aileSyamples 3M ENVIRONMENTALLABORATORY i Note to File ii Project or Study Number: E02-0443 LIMS Number: NA Affected Data: D020812A and D020812B. III II 1. All data that is in D020812A and D020812B are from one original sequence: D020812. The D020812 parent sequence is made up of 161 injections/files. Files DUDE0001 to DUDE0096 are found in the sub-sequence D020812A. Files DUDE0097 to DUDE 0161 are in sub-sequence D020812B. The parent sequence was broken up into two separate sub-sequences after LC/MS analysis to simplify data analysis. Low concentration samples that fall in the bottom end of the standard calibration curve (0.1 ng/mL to 50 ng/mL) are in sub-sequence D020812A. Very high concentration samples that required small injection volumes that fall in the top end of the curve (5 ng/mL to I000 ng/mL) are in sub-sequence D020812B. There are not any files that are contained in both sub-sequences. 2 There are two different extraction dates for the samples: 20 Jun 02 and 17 Jul 02. This is due to a re-extraction of 5 _ampL=swhose results were questionable. 3. The following are the LIMS numbers and the sample names of the samples and their associated duplicates and matrix spikes: 38025 SW01 SW=Sample Water(Sample Location) 38026 38027 SW01-Dup SW01-Low FSC=Field Sample Control FB= Field Blank 38028 38029 38030 38032 38O33 SW01-Med FSC0 l-Low FSC01-Med FB02 SW03 Low=Low Field Spike Med=Medium Field Spike 38034 38035 38036 38037 38038 38039 38340 38041 38042 SW03-Dup SW03-Low SW03-Med SW02 SW02-Dup SW02-Low SW02-Med FCS02-Low FCS02-Med 38043 and 38047 Trip Blank #1 Trip Blank #2 i I IDa II 3MEnvironmentLaal boratory Pageof . Page273 of 276 Report E02-0443 I I II . _ Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY i i|11 i ii m Note to File II I Project or Study Number: E02-0443 LIMS Number: NA Affected Data: D020626Extracted III I 1. In theD020626ExtractesdequencteherewerenotanyExtractedCCVcurvepointsrun. All subsequenFtishTissue sequencehsadextractedCCVsincluded.TheunextracteCdCVswerequantitateadgainsttheunextractefdish curve0, 2003-050,usinganExcelspreadsheeAt.ll of theunextracteCdCVspassedandtheresultsarefoundin Appendix B:Data SummaryTables. 3M Environmental Laboratory Page _ of 6. Page 274 of 276 Report E02-0443 ._ i Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY I Note to File I Project or Study Number: E02-0443 LIMS Number: NA Affected Data: All Data m mill Note: This is to explain how the quantitation wasperformed on the data. 1. The entire calibrationcurve was entered into the quantitationsoftware and the curve was then analyzed. In many cases, high level curve points were "Disabled" in the software and were removed from the curve calculation. In all instances in which this was done, the disabled curve points show a recovery of 0%. Low end curve points that had %Recoveries that exceeded the criteria or were <2X the solvent blanks levels were not used. These points were still included in the calibration curve calculations,however, they were not used in the determination of the LOQ. 2. In the raw data that comes from the Target software, concentrations that would normally be quantitatedas a very low or a negative value are assigned an extreme positive value. These values are easily noticed due to their abnormally large values along with very small area counts. These values, along with values that are below the limit of quantitation, are changed to "BLOQ" to eliminate any possible confusion. 3M EnvironmentalLaboratory Page __ of __... Page 275 of 276 II Report E02-0443 3M ENVIRONMENTAL LABORATORY Note to File . _ Tenn. River Valley Samples Project or Study Number: E02-0443 LIMS Number: NA Affected Data: Fish Tissue In the sample preparationprocessof the fish tissue, afterthe homogenizationprocess(Step4), the homogenate is centxifugedfor a shorttime andthenshaken (Step S). The centrifugatiouwasdoue to elimiuatethe foam that developed during the homogenizationprocess. The homogenatewasthen shaken/vortexedto make the solution homogenous again. 3M Environmental Laboratory Page _. of__. Page 276 of 276